What an amazing route and the quality of the video is amazing, too. I always wanted to make Aspirin with my students but it is not worth the paper work to get acedic anhydride in Europe. thanks for the work putting in on TH-cam. I am impressed!
Okay WAIT, this is so helpful. I have been trying to research how to make acetic anhydride because I was trying to synthesize paracetamol, and I couldn't figure anything out. I don't know how I haven't come across this method but thank you. I sorta gave up on doing a paracetamol lab and moved on to doing testosterone, but now I will do it next thanks to you.
Hello 👋 might I ask if you're trying to synth just the constituents of Paracetamol or the whole compound? I suppose you know that acetaminophen is pretty bad for the liver and can be separated from most opioid/apap combo pills with a simple cold water extraction since the acetaminophen is not water soluble but the opioid is. Good luck in your results.
@@Sniperboy5551 i've heard it can double or quadruple the strength of cannabis too although, of course, that would be a waste. i'd be using it for 'asprin' like you said. 😉
You sound inexperienced, this advice is necessary. Sulfur chlorides are nasty as all hell, not quite 'if you smell it your gonna die' kind of nasty but nasty enough to REQUIRE a fume hood and give you a really bad time, maybe even a headache. Sulfur bromides might be preferable as they are less unwieldy and less volatile, however bromine itself can be a little nasty as well.
@@michaelknight4041 lol,cold water extraction, that brings me back in time. Figured it out from a Merck index in my high school library. Btw, unless it was on the internet before 1996 or 1997 I might have been the first to upload the process.
Awesome video! I'd seen this prep on paper, but wasn't sure if it actually worked. Hell, there's a REALLY long thread on sciencemadness where people were trying literally everything else, I guess they didn't think it was worth trying on a small scale, you proved us wrong.
The thread is so huge particularly because it deals with syntheses using readily available precursors. And the fact that this route isn't bumped should tip you off to the yield here. It's hot garbage. Hot, stinky garbage.
@@amarissimus29 I've talked to a lot of people who figured out the issues with his particular version of this synth and it's actually really high yielding when done properly. You can also distilled sulphur chloride straight from a mix of TCCA and sulfur which cuts down on dirty glassware. Sure it's not going to be adopted for industrial production but it's more than good enough for home chemists unless you're making stuff you probably shouldn't be.
*thinks back to chemistry class being 95% book work* There are so many cool things you can make with basic chemistry. Thanks for sharing your experiences and experiments!
Nauseating to me. I think it has to do with interacting with acetylcholine in the brain, and it may be a genetic susceptibility - vinegar smells absolutely repellant to me, and I don't even like to consume condiments that contain it other than barbecue sauce, but some people love it. The chemicals used to vulcanize the rubber in tires smell delightful to me, as bad as they are for my body, but some people gag when they walk into Discount Tire.
Wow, that was an interesting way to do it. Get the feeling you picked it just so the contaminated sulphur dichloride didn't go to total waste haha xD Loved the gratuitous volcano at the end :)
Omg I've done this before!! I stumbled onto some Wikipedia entry and decided it was possible and made a shtload of sulfur chloride and made about a hundred mLs of Acetic anhydride. I never did test it only observed Acetic anhydrides boiling point and wasn't sure if I did it or not. Now I'm thinking it definitely worked. Thanks for your videos man your channel is very well done.
@@williamackerson_chemist same for me. stored in a nice teflon lined bottle. the teflon just got absolutely ripped apart by the chlorine and sulfur chlorides and the lid got yellow and blistered.
Yeah, but where to get these kgs of Opium? Easier and cheaper to buy the desired product 😂 That's the reason I do not understand why companies don't want to sell these chemicals, as long as they are not illegal (like mentioned in the video)
@@Frank_inSA In Germany there is law called „Grundstoffüberwachungsgesetz“. Yeah that‘s a word an roughly translates to Precursor substance surveillance law. You can’t just buy this as a private person.
@@superman9693 ab 100 Liter bei Essigsäureanhydrid, eigentlich völlig legal in Kleinstmengen, das ist ja genau mein Punkt 😎 Was sollte man denn auch anstellen, mit einem halben Liter? Zumal die Polizei schon kommt, wenn sie eine einzige Mohnblume im Garten sieht 😂 Opium oder gar pures Morphin ist praktisch auch auf dem Schwarzmarkt nicht erhältlich
I almost fainted when I saw you drop your hole yield into water. But I was laughing when you talked about been surprised when it formed a blob on the bottom of the flask. Had exactly the same experience when I dropped some into water and had drops at the button...
This was a new one for me. Clean, simple, surely still dangerous given the chems (if one does it without wisdom) but you definitely schooled us. Now, make a laser diode out of it (or a magnet)😊
Dude another killer video! You're dishing out some great ones! Any chance your organosulfur compound is thioacetic acid(B.P. of 93C)? Or perhaps even the anhydride of thioacetic acid?
sulfur 2 chloride is a normally stable compound (and bright red liquid) . It is sensitive to light because its boiling point is even below the boiling point of water, so above its boiling point, decomposes into sulfur 1 chloride dimer and chlorine. Considering that the light that sublimates iodine will evaporate sulfur 2 chloride, the orange color, even if it is dark, is due to the formation of a small amount of sulfur 1 chloride dimer and its miscibling with the sulfur 2 chloride remaining without decomposition.
When I was studying in University, my friend want to perform one synthesis on organical chemistry class, but it required acetic anhydride. Book with method was soviet and everything was changed. In modern day Russia acetic anhydride is in List 1 or List 2 as precursor and making it (you cannot obtain legally) could cause some severe problems. He had to switch his efforts to a luminol synthesis
I wished you showed diagrams of the compounds and how they are reacting at a given moment at that temperature, would've helped in understanding...... Otherwise, great explanation, nice narration and quite encouraging to watch!
Rather than fusing the wet, hydrated sodium acetate with a torch, MICROWAVE it in a suitable vessel (glass or ceramic and LARGER than you were using here, it will foam & expand as water boils off). Sodiym acetate will stop being heated by microwaves when anhydrous.
oh wow, a reaction we def made , a bunch of, in the 90s. and probably why it is on the watch list now. . LOL but very nice. . @ 02:35 . . i seen that dark liquid, i thought it was starting to tar up or something. However; I was very impressed , that by the next shot, it was that half beaker full of pretty darn clean looking Sodium Acetat *new sub to your channel. very cool projects you have going on for all ages. from high school organic chem students to people like me (45 year olds that have had chem synths in their past lives :) peace,Eurn
Glad you enjoyed it! Yeah, I'm happy to say the darkening of the sodium acetate wasn't too significant, although if I were doing this on a larger scale, I would do what Doug's Lab did and just toss the acetate into the oven, haha!
True, although you'd still need to melt it down to drive off the water. Most instant hot packs use sodium acetate trihydrate, and this react is fairly particular about having anhydrous conditions!
True. The volume of vinegar I had to boil was ridiculous for the yield. I really like how you melted it, that was a gold nugget. I was considering acetyl chloride and acetic acid + ∆ = acetic anhydride + NaCl when I found this vid. There are some S and P compounds I would like to have but I would rather produce than purchase and I have neither element in hand. I have to go back and see how you produced your sulfur chloride.
interesting route to synthesis acetic anhydride, but I HATE working with sulfur compounds 😅(btw I am proud cuz subscribed you when you only have 900 subs)
That would simply yield acetic acid and HCl, which don't interact. If you want acetyl chloride, you'll either have to mix dry HCl gas with acetic anhydride, acetic acid with a dehydrating chlorinating agent (PCl3, PCl5, SOCl2, etc), or an anhydrous acetate with phosphoryl chloride.
If you mean reacting glacial acetic acid with sodium bicarbonate to get the sodium acetate, then yes, that would work (although you'd still need to dry it). But if you're saying refluxing GAA over baking soda to directly make acetic anhydride, then no, that would only produce sodium acetate.
How does this compare to the NO2/sodium acetate method? Also, do you have any suggestions for propionic anhydride? I don't suppose either your method or the NO2 method work with a simple substitution to the propionate version of the sodium's carboxyl piece?
Honestly, I have no idea. I've never tried the NO2 method, but I'd bet that this method is superior simply because you don't have to worry about generating NO2 gas (although if you hate the smell of sulfur chloride like I do, maybe the NO2 route is better). I want to say these methods would work for propionic anhydride, but I'd have to try it for myself to know for sure. Maybe I will someday!
@LabCoatz thanks for the response. And honestly... I'd like to see your take on the NO2 method just because i couldn't really believe it was real. I want to say it popped up in a sciencemadness thread, and then someone on TH-cam tried and verified... I don't recall yields, but it'd be interesting to compare the two routes
Doesn't it suck when you are doing an experiment, and your expected result comes over after a certain temp, but you have nothing left before you get there?...
Hey your glass ware has made in india written on it . When we buy glassware its just the capacity and company's name . I have never seen a glass ware written made in india until now. From where are u bro . Greetings from an Indian.
they probably have to do that for some regulation or importing reason. you know how some governments are. . lol btw. are you living in India now? . . just curious. . ive been there twice from North America and it was amazing both times peace, Eturn
I'm living in central Oklahoma, in the middle of the United States! I bought the beakers from homesciencetools.com, or HST, and I must say, their products hold up excellently!
@@theeturnone ya i am living in india and also producing content like this. But i cant get views. In india this type of content is not being watched . Thats why i am suffering . U can check my channel.
So awesome! Love the videos and information. Man I wish my science classes in high school and college were more hands on/experimental instead of mainly theoretical. Definitely probably would've been safer/on less lists than doing practical experiments on my own at home. Oh well, lol
I don't actually own an adapter to connect tubing with, so I didn't really have a way to send the gases like SO2 through a bubbler trap. I'm hoping to get one soon though!
@Chemistry of Questionable Quality yeah that's how i do it. Stopper the female end and Teflon it and it works great. Or glass tube in a thermometer adapter with hose secured by tape
I've seen that many people who use an SH-2 or SH-3 magnetic stirrer, have removed the oxide coating from their device. Is there any benefit in doing this or was it just that the surface got ruined at one point due to an acid or base spill?
@@LabCoatz_Science Ahh I see. Mine has an Eloxal surface like a Macbook, that's why I was wondering. These devices get built by dozens of different manufacturers, sharing a template or doing reverse engineering by the looks of it. The "brand name" is always another every time I see them. They are absolutely great for the money though, especially for hobbyists!
In terms of materials, this route is much easier for the average person. While you could make benzoyl chloride from OTC chemicals, it's much easier to make sulfur chloride. Sodium acetate is also far more common (and cheaper) than potassium acetate, and it can even be made from plain old vinegar and baking soda like I showed in this video.
Sorry I am Italian and I don't understand, Just to be clear the sulfur monochloride you mention Is cas Number 10025-67-9? Sorry I am kinda Lost in translation
Sulfur chloride is essential. Sulfur trioxide MIGHT work, but it's much harder to get and it would probably just char and decompose the sodium acetate.
@@LabCoatz_Science yeah, I’ve tried to separate combining methods because I’m just making what I need and I’m just not getting something right. I don’t have the glass tube for the surfer powder.
Just so you know, sulfur monochloride is light golden yellow - it it's orange atl all, you have excess chlorine and soime sulfur dichloride.. Making this stuff from sulfur and chlorine normally requires you distill the crude product over excess sulfur to get the actual monochloride. just fwiw.
Yeah, I know. It was a lot more yellow in person, but the video showed it as more of a red. To be safe, I would've done a reflux over sulfur, but I wasn't in the mood to mess with the sulfur chlorides more than I had to, lol!
Sulfur monochloride or sulfur dichloride. You say one and another is on the bottle. Can you please clarify? Also Backyard Science no longer has this listed 😢
Not sure where you heard that, but that's actually the exact opposite of what happens: whenever acetic anhydride is exposed to air, it reacts with the moisture to form acetic acid (which is why it tends to smell like vinegar).
Can you make acetic anhydride by dehydrating acetic acid with phosphorus pentoxide, like you can make sulfur trioxide by dehydrating sulfuric acid with phosphorus pentoxide?
Yeah, unfortunately Backyard Science 2000 decided to close down after trouble with eBay and some other stuff. There are other sellers though, such as Chemsavers.com (looks like they offer 500mL for $66 currently, and they will ship most items to residential addresses).
An aspirator beats the hell out of a vacuum pump in situations like this, so there's really no excuse for not pulling a vacuum. You don't have to worry about destroying components and scrubbing is simplified as well. Horrible, nasty looking reactions can look like boiling water under the right conditions. And aspirators are dirt cheap.
Acetic acid's boiling point is very close to that of water, so separating it via distillation would be very difficult. In theory though, you could probably distill off some of the water to get a more concentrated acid, but I doubt you could achieve 100% acetic acid in this way. Overall, the best way to get pure acetic acid is by neutralizing vinegar with baking soda, boiling away all of the water, and then acidifying the resulting sodium acetate with sulfuric acid.
Love seeing the channel grow. If you’re in the US, do you know the regulations regarding smaller research amounts of energetics? To me it seems like you’re not really supposed to touch any of that without a license so I was actually considering getting an ATF license just to make very small quantities for videos and research. I’m doing a cubane project right now and I would like to make some different types of cubane. The priority is regular cubane, then trying perfluorocubane, then taking a crack at energetic cubanes. I just don’t want to get into any hot water especially because of posting videos.
Thanks! I don't know the exact regulations, but it seems that you do need an ATF license to work with explosives of any quantity. I know channels like DBX Labs and ReactiveChem that shut down their energetics projects (very small scale, only a few milligrams at a time) because they got raided by the government. Moral of the story: don't post yourself making explosives on TH-cam without a license, haha! Although, I'm sure there are some excusable ways around this...like in my video about manganese heptoxide, I mixed the heptoxide with magnesium and got a detonation. Probably won't get a visit for that one because it was (mostly) an accident, and I didn't TECHNICALLY manufacture an explosive.
Technically you can make explosives as long as you don't do it in a residence, don't store, transport, sell, or make money off their use (this includes TH-cam money). Darian Ballard has been visited and was totally within the law, he continues to make energetics videos. The other guys technically violated the law, but luckily didn't get in any trouble (the ATF isn't always known for being reasonable or following the law). I've had public safety Canada and CSIS ask friends about me and my chemistry interests, as well as my politics, neither of which are illegal. I don't talk to cops generally, but if you look at your local and federal laws and follow them you should be ok.
@@chemistryofquestionablequa6252 That’s what I kind of gathered from reading all of the ATF stuff was that generally the licenses were for businesses. Like the manufacturer license is a manufacturer AND sale license. The laws in the US can be so unbelievably confusing and at times can be interpreted entirely differently depending on who you ask so it can be frustrating. Thanks for the info!
@@LabCoatz_Science well that’s fun. It’s like $200/yr and I’m sure they’re not easy to get. Will have to look into it some more. Will share info if I come across something. Looking forward to your next project already good sir!
@@MaxfieldMED ATF licencing isn't hard to get. Mostly just costs you large amounts of time and a little money (assuming you already have a safe storage location for the energetics. Obv building an ordnance magazine can be costly if you don't have one on hand). But citizens should think carefully before giving federal agencies permission to "audit" their homes and places of business. Best to avoid that relationship unless you absolutely HAVE to get into it.
No, in that case, you'd get potassium chloride and benzoyl acetate. You could get the anhydride from acetyl chloride and an acetate though (since acetyl acetate is acetic anhydride).
@@kemalk-gt7cu Why do you care so much? Acetyl chloride is way harder to get than the chemicals I used, and it would still require a distillation (assuming you're still trying to avoid that). If you really want to know the formulas and all that, look up Thy Labs' video on making acetic anhydride from acetyl chloride, or check Wikipedia.
Cool, I would do this if I didn't already have acetic anhydride. I'd welcome any other synthesis using sulfur monochloride, not necessarily to make CS2... 😜
It was much cheaper. Although there is less acetic acid overall in 5% vinegar, I can get a gallon for $3 while a gallon of 30% "cleaner/weed killer-grade" vinegar is $20, so I never really spent the money to get the extra-strength stuff. Plus, I usually have 5% around the house, so it was easier to just grab-and-go!
If you're asking if you can get acetic anhydride using this method without distillation, then no. The result is a crumbly paste of sulfur, sulfur compounds, salt, and acetic anhydride, and it must be heated at 100C either way to drive the reaction to completion. It isn't liquid enough to simply pour/filter off the anhydride.
Acetic anhydride synthesis + molecules in intro: ethylphenidate, some weird methylenedioxy-dimethyl-cathinone (edit: found it, dibutylone), are you researching better alternatives for your ADHD medication?
Make sure you make grade 4 pure Burmese type Heroin not like that worthless Afghan heroin grqde 3. We need grade 4 heroin. Burmese Heroin Double Globe.
@@LabCoatz_Science That's from book named Синтетические химико-фармацевтические препараты, author's surname Кацнельсон. Quite old book, printed exactly a century ago
Comes under any type of these videos 😢 Thing is, where do you get the morphine or raw opium from? Much easier to buy the desired end product, I don't understand the bo-hoo about acetic anhydride. Of course, if you live in Mexiko or Afghanistan.....
No, acetic acid doesn't spontaneously lose water and become the anhydride. To get acetic anhydride from pure acetic acid, you'd need a fairly aggressive dehydrating agent, like phosphorus pentoxide.
@@kemalk-gt7cu Yes, using the way I showed in this video. Or, if you have acetyl chloride on hand for some reason, you could react that with sodium acetate instead of sulfur chloride.
@@LabCoatz_Science good to hear! Luckily I do have access to AcCl but last time I worked with I realized I‘d rather not work with it again in a shoddy home lab
Your video quality is getting pretty awesome man.
Thanks man, glad you enjoyed the video!
@@LabCoatz_Sciencecan this be done with pure acetic acid instead of distilling the vinegar?
What an amazing route and the quality of the video is amazing, too. I always wanted to make Aspirin with my students but it is not worth the paper work to get acedic anhydride in Europe. thanks for the work putting in on TH-cam. I am impressed!
Nice! Didn't know this route would even be useful in an amateur setting but you proved it is.
I tried this procedure a while back and failed, it's good to see a video on this route to acetic anhydride. Good job!
I've never seen such a unique and cool sponsor for a video - and even funnier he does ASMR videos, lol.
What a world we live in 🤔
This is actually an extremely helpful way on how to make acetic anhydride and very easy and cost effective
Awesome video! The production quality was top notch!
Thanks man, glad you liked it!
Extra props to backyardscience 2000!!! Solid seller. Bought like 3 helpings of his aminoguanadine bicarbonate when I was messing about with tetrazoles
Okay WAIT, this is so helpful. I have been trying to research how to make acetic anhydride because I was trying to synthesize paracetamol, and I couldn't figure anything out. I don't know how I haven't come across this method but thank you. I sorta gave up on doing a paracetamol lab and moved on to doing testosterone, but now I will do it next thanks to you.
Hello 👋 might I ask if you're trying to synth just the constituents of Paracetamol or the whole compound? I suppose you know that acetaminophen is pretty bad for the liver and can be separated from most opioid/apap combo pills with a simple cold water extraction since the acetaminophen is not water soluble but the opioid is. Good luck in your results.
Acetic anhydride is more useful for an aspirin (or heroin) synthesis
@@Sniperboy5551 i've heard it can double or quadruple the strength of cannabis too although, of course, that would be a waste. i'd be using it for 'asprin' like you said. 😉
You sound inexperienced, this advice is necessary.
Sulfur chlorides are nasty as all hell, not quite 'if you smell it your gonna die' kind of nasty but nasty enough to REQUIRE a fume hood and give you a really bad time, maybe even a headache.
Sulfur bromides might be preferable as they are less unwieldy and less volatile, however bromine itself can be a little nasty as well.
@@michaelknight4041 lol,cold water extraction, that brings me back in time. Figured it out from a Merck index in my high school library. Btw, unless it was on the internet before 1996 or 1997 I might have been the first to upload the process.
Awesome video! I'd seen this prep on paper, but wasn't sure if it actually worked. Hell, there's a REALLY long thread on sciencemadness where people were trying literally everything else, I guess they didn't think it was worth trying on a small scale, you proved us wrong.
The thread is so huge particularly because it deals with syntheses using readily available precursors. And the fact that this route isn't bumped should tip you off to the yield here. It's hot garbage. Hot, stinky garbage.
@@amarissimus29 I've talked to a lot of people who figured out the issues with his particular version of this synth and it's actually really high yielding when done properly. You can also distilled sulphur chloride straight from a mix of TCCA and sulfur which cuts down on dirty glassware. Sure it's not going to be adopted for industrial production but it's more than good enough for home chemists unless you're making stuff you probably shouldn't be.
this is actually a pretty good way to generate SO2 as well - if you don't have any bisulfite for some reason
I'm struggling to decide whether death by ketene is worse than death by organo-sulfurous stench overwhelm.
*thinks back to chemistry class being 95% book work*
There are so many cool things you can make with basic chemistry. Thanks for sharing your experiences and experiments!
Yeah, I'm saving this one.
This stuff smells so good. Its a bit of a shock the first few times but god I love vinegarish smells
Nauseating to me. I think it has to do with interacting with acetylcholine in the brain, and it may be a genetic susceptibility - vinegar smells absolutely repellant to me, and I don't even like to consume condiments that contain it other than barbecue sauce, but some people love it. The chemicals used to vulcanize the rubber in tires smell delightful to me, as bad as they are for my body, but some people gag when they walk into Discount Tire.
Wow, that was an interesting way to do it. Get the feeling you picked it just so the contaminated sulphur dichloride didn't go to total waste haha xD Loved the gratuitous volcano at the end :)
Yeah, the sulfur chlorides had to go, lol
Omg I've done this before!! I stumbled onto some Wikipedia entry and decided it was possible and made a shtload of sulfur chloride and made about a hundred mLs of Acetic anhydride.
I never did test it only observed Acetic anhydrides boiling point and wasn't sure if I did it or not. Now I'm thinking it definitely worked. Thanks for your videos man your channel is very well done.
Oh and my plastic lid did the exact same thing as yours. You cannot just store sulfur monochloride outside an ampule despite what it may tell you
@@williamackerson_chemist same for me. stored in a nice teflon lined bottle. the teflon just got absolutely ripped apart by the chlorine and sulfur chlorides and the lid got yellow and blistered.
Chemistry was the hardest science branch I studied at university. I learned a lot.👨🎓
Awesome! Now I can make my own H! 👍
Hah,glad I'm not the only one who's thinking along those lines..Those sticky dark beetle lines
Yeah, but where to get these kgs of Opium?
Easier and cheaper to buy the desired product 😂
That's the reason I do not understand why companies don't want to sell these chemicals, as long as they are not illegal (like mentioned in the video)
@@Frank_inSA In Germany there is law called „Grundstoffüberwachungsgesetz“. Yeah that‘s a word an roughly translates to Precursor substance surveillance law.
You can’t just buy this as a private person.
@@superman9693 ab 100 Liter bei Essigsäureanhydrid, eigentlich völlig legal in Kleinstmengen, das ist ja genau mein Punkt 😎
Was sollte man denn auch anstellen, mit einem halben Liter? Zumal die Polizei schon kommt, wenn sie eine einzige Mohnblume im Garten sieht 😂
Opium oder gar pures Morphin ist praktisch auch auf dem Schwarzmarkt nicht erhältlich
@Frank_inSA it ain't easy to find h anymore which is super unfortunate lol
You are THE MAN!!!
Great video.also a cool sponsor to have
I almost fainted when I saw you drop your hole yield into water.
But I was laughing when you talked about been surprised when it formed a blob on the bottom of the flask. Had exactly the same experience when I dropped some into water and had drops at the button...
That's how you know it's legit! Not the most practical way to make vinegar though.
This was a new one for me. Clean, simple, surely still dangerous given the chems (if one does it without wisdom) but you definitely schooled us. Now, make a laser diode out of it (or a magnet)😊
You can be the next nile red! You are great.
A really good video! Keep it up!
Not looking forward to working with S2Cl2 again
Gotta hate the sulfur chlorides man! They stink worse than thioacetone, imo!
Dude another killer video! You're dishing out some great ones! Any chance your organosulfur compound is thioacetic acid(B.P. of 93C)? Or perhaps even the anhydride of thioacetic acid?
It's very possible, good thought!
sulfur 2 chloride is a normally stable compound (and bright red liquid) . It is sensitive to light because its boiling point is even below the boiling point of water, so above its boiling point, decomposes into sulfur 1 chloride dimer and chlorine. Considering that the light that sublimates iodine will evaporate sulfur 2 chloride, the orange color, even if it is dark, is due to the formation of a small amount of sulfur 1 chloride dimer and its miscibling with the sulfur 2 chloride remaining without decomposition.
i would have given my eye-teeth for this video a few years ago but i'm a good boy now!
Blaming your eggy farts on the sulfure chlorides. Nice one, bro. Not many have this kind of logical inputs in their productions!
superb job. you get my vote
New sub. I just like listening to you talk.
I've made it. Good for polymers. Yup don't overheat, or you'll get sodium triacetate.
When I was studying in University, my friend want to perform one synthesis on organical chemistry class, but it required acetic anhydride. Book with method was soviet and everything was changed. In modern day Russia acetic anhydride is in List 1 or List 2 as precursor and making it (you cannot obtain legally) could cause some severe problems. He had to switch his efforts to a luminol synthesis
lovely
I wished you showed diagrams of the compounds and how they are reacting at a given moment at that temperature, would've helped in understanding......
Otherwise, great explanation, nice narration and quite encouraging to watch!
I know how bad that vinegar smelled as it boiled. Cool video!!
This was amazing
Backyardscience 2000 gigachad
Now i'd like to know how to turn poppy plants into dia m orphine
You got at least an acre where you can plant poppies? 😂
Btw, there is an old DEA publication to be found on the web, describing the process in detail.
You're going to bet at 100 thousand subs in no time.
to really purify the sodium acetate it can be recrystallized in methanol hydrate, I have done this multiple times for making glacial acetic acid.
Rather than fusing the wet, hydrated sodium acetate with a torch, MICROWAVE it in a suitable vessel (glass or ceramic and LARGER than you were using here, it will foam & expand as water boils off). Sodiym acetate will stop being heated by microwaves when anhydrous.
oh wow, a reaction we def made , a bunch of, in the 90s. and probably why it is on the watch list now. . LOL
but very nice. . @ 02:35 . . i seen that dark liquid, i thought it was starting to tar up or something.
However;
I was very impressed , that by the next shot, it was that half beaker full of pretty darn clean looking Sodium Acetat
*new sub to your channel. very cool projects you have going on for all ages. from high school organic chem students to people like me (45 year olds that have had chem synths in their past lives :)
peace,Eurn
Glad you enjoyed it! Yeah, I'm happy to say the darkening of the sodium acetate wasn't too significant, although if I were doing this on a larger scale, I would do what Doug's Lab did and just toss the acetate into the oven, haha!
not common to see a disulfide linkage but you cant really expect the sulfur and organics to not smell i guess
Could you please also synthesize phthalic acid (and then phthalic anhydride) from naphthalene ?
Convenient starting point to get sodium acetate without the day of boiling is to open an instant heat pack, the kind you snap to activate.
True, although you'd still need to melt it down to drive off the water. Most instant hot packs use sodium acetate trihydrate, and this react is fairly particular about having anhydrous conditions!
True. The volume of vinegar I had to boil was ridiculous for the yield. I really like how you melted it, that was a gold nugget. I was considering acetyl chloride and acetic acid + ∆ = acetic anhydride + NaCl when I found this vid. There are some S and P compounds I would like to have but I would rather produce than purchase and I have neither element in hand. I have to go back and see how you produced your sulfur chloride.
interesting route to synthesis acetic anhydride, but I HATE working with sulfur compounds 😅(btw I am proud cuz subscribed you when you only have 900 subs)
It's crazy what you can buy if you don't mind being on a list.
If you have anhydrous sodium acetate mixed with dried sodium chloride couldn’t you add Reagant grade sulfuric acid to make acetyl chloride?
That would simply yield acetic acid and HCl, which don't interact. If you want acetyl chloride, you'll either have to mix dry HCl gas with acetic anhydride, acetic acid with a dehydrating chlorinating agent (PCl3, PCl5, SOCl2, etc), or an anhydrous acetate with phosphoryl chloride.
Can I use anhydrous glacial acetic acid? Refluxing baking soda with GAA and later evaporating is enough. Am I right?
If you mean reacting glacial acetic acid with sodium bicarbonate to get the sodium acetate, then yes, that would work (although you'd still need to dry it). But if you're saying refluxing GAA over baking soda to directly make acetic anhydride, then no, that would only produce sodium acetate.
@@LabCoatz_Science please your Instagram I will follow you
7:47 Tom from Extractions&Ire called.
can you please measure the amount of mercury in fish? various brands/species from a grocery store
gotta love acetic anhydride
Cackled at the circle of life audio
How does this compare to the NO2/sodium acetate method?
Also, do you have any suggestions for propionic anhydride? I don't suppose either your method or the NO2 method work with a simple substitution to the propionate version of the sodium's carboxyl piece?
Honestly, I have no idea. I've never tried the NO2 method, but I'd bet that this method is superior simply because you don't have to worry about generating NO2 gas (although if you hate the smell of sulfur chloride like I do, maybe the NO2 route is better). I want to say these methods would work for propionic anhydride, but I'd have to try it for myself to know for sure. Maybe I will someday!
@LabCoatz thanks for the response. And honestly... I'd like to see your take on the NO2 method just because i couldn't really believe it was real. I want to say it popped up in a sciencemadness thread, and then someone on TH-cam tried and verified... I don't recall yields, but it'd be interesting to compare the two routes
Can i use sodium carbonate since thats all i have at the moment?
Doesn't it suck when you are doing an experiment, and your expected result comes over after a certain temp, but you have nothing left before you get there?...
Oh how neat was the mishap with the plastic lid 😂
Hey your glass ware has made in india written on it . When we buy glassware its just the capacity and company's name . I have never seen a glass ware written made in india until now. From where are u bro .
Greetings from an Indian.
they probably have to do that for some regulation or importing reason. you know how some governments are. . lol
btw. are you living in India now? . . just curious. . ive been there twice from North America and it was amazing both times
peace, Eturn
I'm living in central Oklahoma, in the middle of the United States! I bought the beakers from homesciencetools.com, or HST, and I must say, their products hold up excellently!
@@LabCoatz_Science oh nice .
@@theeturnone ya i am living in india and also producing content like this.
But i cant get views. In india this type of content is not being watched . Thats why i am suffering .
U can check my channel.
i think my brain paused in crushed expectations there was no cod hitmarker on the drop spilled at 6:49 lol
So awesome! Love the videos and information.
Man I wish my science classes in high school and college were more hands on/experimental instead of mainly theoretical.
Definitely probably would've been safer/on less lists than doing practical experiments on my own at home.
Oh well, lol
Any reason you didn't use a bleach/permanganate trap during reflux? Seems like that would make this prep way nicer
I don't actually own an adapter to connect tubing with, so I didn't really have a way to send the gases like SO2 through a bubbler trap. I'm hoping to get one soon though!
@@LabCoatz_Science use a vacuum take off adapter with a glove rubber banded over the open joint. You have one if you have a distillation apparatus.
@Chemistry of Questionable Quality yeah that's how i do it. Stopper the female end and Teflon it and it works great. Or glass tube in a thermometer adapter with hose secured by tape
Hahaha love the anecdote for elementary students, I definitely was the kid throwing all of it in for the eruption😂
I've seen that many people who use an SH-2 or SH-3 magnetic stirrer, have removed the oxide coating from their device. Is there any benefit in doing this or was it just that the surface got ruined at one point due to an acid or base spill?
My stirrer always had a metallic finish, although it has gotten a bit messed up over the years from chemical exposure
@@LabCoatz_Science Ahh I see. Mine has an Eloxal surface like a Macbook, that's why I was wondering.
These devices get built by dozens of different manufacturers, sharing a template or doing reverse engineering by the looks of it. The "brand name" is always another every time I see them. They are absolutely great for the money though, especially for hobbyists!
It will melt the teflon off the stir bar.
The first route with potassiumacetat and Benzoyl chloride would be an possible too. I think its easier. Special to make the Benzoyl chloride
In terms of materials, this route is much easier for the average person. While you could make benzoyl chloride from OTC chemicals, it's much easier to make sulfur chloride. Sodium acetate is also far more common (and cheaper) than potassium acetate, and it can even be made from plain old vinegar and baking soda like I showed in this video.
2:37 Got me scared for a moment. It has the color of Tar.
Have a great day!
What is the time and minimum temperature needed for acetylation without solvent?
You'd have to be way more specific, since acetylations conditions depend on what you're acetylating.
Sorry I am Italian and I don't understand, Just to be clear the sulfur monochloride you mention Is cas Number 10025-67-9? Sorry I am kinda Lost in translation
Yes, that is correct. I made it myself in an older video by reacting hot sulfur with chlorine gas.
Do I have to use soap for mono chloride or with any sold for derivative work
Sulfur chloride is essential. Sulfur trioxide MIGHT work, but it's much harder to get and it would probably just char and decompose the sodium acetate.
@@LabCoatz_Science yeah, I’ve tried to separate combining methods because I’m just making what I need and I’m just not getting something right. I don’t have the glass tube for the surfer powder.
Just so you know, sulfur monochloride is light golden yellow - it it's orange atl all, you have excess chlorine and soime sulfur dichloride.. Making this stuff from sulfur and chlorine normally requires you distill the crude product over excess sulfur to get the actual monochloride. just fwiw.
Yeah, I know. It was a lot more yellow in person, but the video showed it as more of a red. To be safe, I would've done a reflux over sulfur, but I wasn't in the mood to mess with the sulfur chlorides more than I had to, lol!
Sulfur monochloride or sulfur dichloride. You say one and another is on the bottle. Can you please clarify? Also Backyard Science no longer has this listed 😢
Sulfur monochloride is recommended, but sulfur dichloride might also work.
"A healthy dose of nasty sulphur chlorides", never heard that one before
I've heard that acetic anhydride is formed when acetic acid reacts with moisture in the air.
Not sure where you heard that, but that's actually the exact opposite of what happens: whenever acetic anhydride is exposed to air, it reacts with the moisture to form acetic acid (which is why it tends to smell like vinegar).
MomCoatz doesn’t trust sulfur monochloride either 👀
No she does NOT, and for good reason!
Can you make acetic anhydride by dehydrating acetic acid with phosphorus pentoxide, like you can make sulfur trioxide by dehydrating sulfuric acid with phosphorus pentoxide?
Yes, you should be able to.
you official inventory list on the google drive is a broken hyperlink.
Yeah, unfortunately Backyard Science 2000 decided to close down after trouble with eBay and some other stuff. There are other sellers though, such as Chemsavers.com (looks like they offer 500mL for $66 currently, and they will ship most items to residential addresses).
🔥
wow backyard science 2000 really gets around huh? love the circle of life joke
An aspirator beats the hell out of a vacuum pump in situations like this, so there's really no excuse for not pulling a vacuum. You don't have to worry about destroying components and scrubbing is simplified as well. Horrible, nasty looking reactions can look like boiling water under the right conditions. And aspirators are dirt cheap.
Can someone explain to someone who's dumb like me, why your can't distill to higher acetic acid concentration then dry using like drying agents
Acetic acid's boiling point is very close to that of water, so separating it via distillation would be very difficult. In theory though, you could probably distill off some of the water to get a more concentrated acid, but I doubt you could achieve 100% acetic acid in this way. Overall, the best way to get pure acetic acid is by neutralizing vinegar with baking soda, boiling away all of the water, and then acidifying the resulting sodium acetate with sulfuric acid.
Just add morphine .
Love seeing the channel grow. If you’re in the US, do you know the regulations regarding smaller research amounts of energetics? To me it seems like you’re not really supposed to touch any of that without a license so I was actually considering getting an ATF license just to make very small quantities for videos and research. I’m doing a cubane project right now and I would like to make some different types of cubane. The priority is regular cubane, then trying perfluorocubane, then taking a crack at energetic cubanes. I just don’t want to get into any hot water especially because of posting videos.
Thanks! I don't know the exact regulations, but it seems that you do need an ATF license to work with explosives of any quantity. I know channels like DBX Labs and ReactiveChem that shut down their energetics projects (very small scale, only a few milligrams at a time) because they got raided by the government. Moral of the story: don't post yourself making explosives on TH-cam without a license, haha! Although, I'm sure there are some excusable ways around this...like in my video about manganese heptoxide, I mixed the heptoxide with magnesium and got a detonation. Probably won't get a visit for that one because it was (mostly) an accident, and I didn't TECHNICALLY manufacture an explosive.
Technically you can make explosives as long as you don't do it in a residence, don't store, transport, sell, or make money off their use (this includes TH-cam money). Darian Ballard has been visited and was totally within the law, he continues to make energetics videos. The other guys technically violated the law, but luckily didn't get in any trouble (the ATF isn't always known for being reasonable or following the law). I've had public safety Canada and CSIS ask friends about me and my chemistry interests, as well as my politics, neither of which are illegal. I don't talk to cops generally, but if you look at your local and federal laws and follow them you should be ok.
@@chemistryofquestionablequa6252 That’s what I kind of gathered from reading all of the ATF stuff was that generally the licenses were for businesses. Like the manufacturer license is a manufacturer AND sale license. The laws in the US can be so unbelievably confusing and at times can be interpreted entirely differently depending on who you ask so it can be frustrating. Thanks for the info!
@@LabCoatz_Science well that’s fun. It’s like $200/yr and I’m sure they’re not easy to get. Will have to look into it some more. Will share info if I come across something. Looking forward to your next project already good sir!
@@MaxfieldMED ATF licencing isn't hard to get. Mostly just costs you large amounts of time and a little money (assuming you already have a safe storage location for the energetics. Obv building an ordnance magazine can be costly if you don't have one on hand). But citizens should think carefully before giving federal agencies permission to "audit" their homes and places of business. Best to avoid that relationship unless you absolutely HAVE to get into it.
Can it be done by heating potassium acetate and benzoyl chloride?
No, in that case, you'd get potassium chloride and benzoyl acetate. You could get the anhydride from acetyl chloride and an acetate though (since acetyl acetate is acetic anhydride).
@@LabCoatz_Science can you give me the exact formulas
@@kemalk-gt7cu Why do you care so much? Acetyl chloride is way harder to get than the chemicals I used, and it would still require a distillation (assuming you're still trying to avoid that). If you really want to know the formulas and all that, look up Thy Labs' video on making acetic anhydride from acetyl chloride, or check Wikipedia.
@@LabCoatz_Science but what is acetyl chloride used for?
Cool, I would do this if I didn't already have acetic anhydride. I'd welcome any other synthesis using sulfur monochloride, not necessarily to make CS2... 😜
Why using 5% vinegar? In my country, you can buy 25% concentrated vinegar in the supermarket.
It was much cheaper. Although there is less acetic acid overall in 5% vinegar, I can get a gallon for $3 while a gallon of 30% "cleaner/weed killer-grade" vinegar is $20, so I never really spent the money to get the extra-strength stuff. Plus, I usually have 5% around the house, so it was easier to just grab-and-go!
Can't we do it by adding it if it's not distillation?
If you're asking if you can get acetic anhydride using this method without distillation, then no. The result is a crumbly paste of sulfur, sulfur compounds, salt, and acetic anhydride, and it must be heated at 100C either way to drive the reaction to completion. It isn't liquid enough to simply pour/filter off the anhydride.
Acetic anhydride synthesis + molecules in intro: ethylphenidate, some weird methylenedioxy-dimethyl-cathinone (edit: found it, dibutylone), are you researching better alternatives for your ADHD medication?
I Was making heroin from poppy pods I stole, thanks this was useful.
Make a review on your process pls asking for a friend
Make sure you make grade 4 pure Burmese type Heroin not like that worthless Afghan heroin grqde 3. We need grade 4 heroin. Burmese Heroin Double Globe.
Do you have a citation for the literature you followed for this procedure?
Just this sketchy Swiss website: chemistry.mdma.ch/hiveboard/rhodium/anhydrides.html
@@LabCoatz_Science lmao only slightly sketch
@@LabCoatz_Science That's from book named Синтетические химико-фармацевтические препараты, author's surname Кацнельсон. Quite old book, printed exactly a century ago
Remarkable….We make it routinely from Sodium Acetate and Acetyl Chloride. Much easier….
Acetyl chloride is so difficult to obtain that it defeats the purpose though.
Can you make hydrazine next?
I already have a nice sample of hydrazine sulfate, so I might try to make anhydrous hydrazine from it sometime in the future, as well as a few azides!
Great! Now I can turn my poppy plants into Heroin!
Lol, I feel like arsenic is hard to find for a good reason!
I would rather make acetyl chloride myself then do sulfur chloride torture xD. Not everyone has access to PCl5 like I do tho. Still a great vid.
Sulfur monochloride is pretty nice thing to work with, POCl3 is much less favorable one. Don't waste your PCl5 on shitty synthesises like this one(
@@dimaminiailo3723 I was half-joking. Trying to produce acetic anhydride by myself can get me in court in my country.
@@I_XuMuK_I Yea Russia is something like that
@@dimaminiailo3723 I'm not in russia
Fun fact: acetic anhydride is used to acetylate morphine and make Diacetylmorphine (heroin).
Comes under any type of these videos 😢
Thing is, where do you get the morphine or raw opium from? Much easier to buy the desired end product, I don't understand the bo-hoo about acetic anhydride.
Of course, if you live in Mexiko or Afghanistan.....
"never trust sulfur chlorides" thinking about Ex&F Tom's S4N4 synthesis
Love the content. I recommend significantly lowering the intro music volume... that wasn't fun at all.
Isn't acetic anhydride formed spontaneously by adding acetic acid to something? easier way
No, acetic acid doesn't spontaneously lose water and become the anhydride. To get acetic anhydride from pure acetic acid, you'd need a fairly aggressive dehydrating agent, like phosphorus pentoxide.
@@LabCoatz_Science without using phosphorus pentoxide
Can it be made any other way than acetic acid?
@@kemalk-gt7cu Yes, using the way I showed in this video. Or, if you have acetyl chloride on hand for some reason, you could react that with sodium acetate instead of sulfur chloride.
BYS 2000 sadly doesnt have AcAnh anymore :(
He's always restocking though! 😉
@@LabCoatz_Science good to hear! Luckily I do have access to AcCl but last time I worked with I realized I‘d rather not work with it again in a shoddy home lab
Damn thats a lot of work, ill keep buying aspirin i guess😂