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Very nice! I caught this on Youtube earlier, same high quality as always. I just can't f-ing BELIEVE that this can stay up publicly on youtube of all platforms though? I mean, chemplayer got taken down for even mentioning P2P in his videos. Beyond the production value and instructional quality of your videos, that itself is an amazing achievement! :).
But that aside, great job as always! This one is maybe a liiiittle bit too roughly and quickly edited though, sometimes it's a bit hard to keep up with which solution is which. Not a problem if one just concentrates and watches it in portions though.
 
, chemplayer got taken down for even mentioning P2P in his videos.

the username you choose is very important on youtube.

personal I would just post a trailer on youtube and redirect people to this platform
 
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Very nice! I caught this on Youtube earlier, same high quality as always. I just can't f-ing BELIEVE that this can stay up publicly on youtube of all platforms though? I mean, chemplayer got taken down for even mentioning P2P in his videos. Beyond the production value and instructional quality of your videos, that itself is an amazing achievement! :).
But that aside, great job as always! This one is maybe a liiiittle bit too roughly and quickly edited though, sometimes it's a bit hard to keep up with which solution is which. Not a problem if one just concentrates and watches it in portions though.
We expect that our channel will also be deleted sooner or later, so all videos are duplicated on the forum. Download them to yourself, sooner or later they will be hard to find. I don't think anyone would be willing as we are to invest as much effort and resources in creating such a high quality video on the subject of syntheses.
 
H
We expect that our channel will also be deleted sooner or later, so all videos are duplicated on the forum. Download them to yourself, sooner or later they will be hard to find. I don't think anyone would be willing as we are to invest as much effort and resources in creating such a high quality video on the subject of syntheses.
How true.
 
We expect that our channel will also be deleted sooner or later, so all videos are duplicated on the forum. Download them to yourself, sooner or later they will be hard to find. I don't think anyone would be willing as we are to invest as much effort and resources in creating such a high quality video on the subject of syntheses.
True. Definitely the highest quality videos I've ever seen on the topic of clandestine chemistry on ANY theme. The fact that it's about drug production makes it absolutely awesome.
 
I have been waiting for this! nice video. A couple of questions:
One of the necks on three neck flask is used for the overhead stirrer, another is used for the additions and the last one is for the thermometer and "has to be opened and directed to a fume hood" if one does not have access to a fume hood, can't one of the necks instead be used for a hose that redirects the gas elsewhere and leave the thermometer?
And to do this can't you just use a stir bar instead of the overhead stirrer? Even if you have to scale the reaction down?
 
I have been waiting for this! nice video. A couple of questions:
One of the necks on three neck flask is used for the overhead stirrer, another is used for the additions and the last one is for the thermometer and "has to be opened and directed to a fume hood" if one does not have access to a fume hood, can't one of the necks instead be used for a hose that redirects the gas elsewhere and leave the thermometer?
And to do this can't you just use a stir bar instead of the overhead stirrer? Even if you have to scale the reaction down?
I have done it using a stir bar, the reaction nicely scales down. Just be careful before adding the CuCl2. This should be done in as short time as possible but keeping the temperature under 80C so prepare a reflux (even a splash head if you have one) and an ice bath. The reflux should also have very cold water circulating. Initially I had some splashing when the foaming got too violent, but this can be managed by waiting enough time between each addition. Also, the best is to attach a receiving flask/hose or anything to direct the any accidental splash into. This can then be added back to the reaction mix. I think the addition in the video is too slow and yield could be better with a more adventurous addition, but this needs to be prepared properly. There is a good post here by a user named eidolon, I think his advice is spot on. This might not be so easily doable on a large scale, but up to a 100g P2NP it is definitely doable.
 
Good morning everyone!!!
First, congratulate Adm for his dedication to creating this channel, everything is amazing and professional, thank you!!!

I'm from Brazil,
I sell cocaine locally, I would like to expand, start selling online, please, anyone who can send me tips, I appreciate it....
 
There was a lot of controversy on this topic 20 years ago.
on the hive, on the hyperlab, on the erovid, in the literature on chemistry.
nowhere and never have I seen nitropropene reduced with sodium borohydride so easily and in high yields.
I'm not 100% sure.
but in my opinion all this is doubtful and may be a fake.
though it looks impressive.
I know that transition metal salts can be catalysts for such reductions.
but I have not seen such a reaction with such good outputs anywhere, I think if it worked, then everyone would have known about it for a long time.
in the classic formulation of rhodium, sodium borohydride can be used to reduce nitrostyrenes to phenethylamines with a normal preparative yield of the reaction product.
but never, on any site, anywhere and no one over the past 20 years has said that borohydride can reduce nitropropenes in high yields in the same way.
It turns out a dilemma.
Everything looks great and the video is of good quality, but judging by other sources, this cannot be.

P.S. I hope I'm wrong and it really works, because the video looks very impressive.
 
Everything looks great and the video is of good quality, but judging by other sources, this cannot be.
I hasten to notice that there is very little relevant and up-to-date information on the Internet. Therefore speaking about other sources - they are all outdated and irrelevant. It is necessary to keep up with the times.
 
There was a lot of controversy on this topic 20 years ago.
on the hive, on the hyperlab, on the erovid, in the literature on chemistry.
nowhere and never have I seen nitropropene reduced with sodium borohydride so easily and in high yields.
I'm not 100% sure.
but in my opinion all this is doubtful and may be a fake.
though it looks impressive.
I know that transition metal salts can be catalysts for such reductions.
but I have not seen such a reaction with such good outputs anywhere, I think if it worked, then everyone would have known about it for a long time.
in the classic formulation of rhodium, sodium borohydride can be used to reduce nitrostyrenes to phenethylamines with a normal preparative yield of the reaction product.
but never, on any site, anywhere and no one over the past 20 years has said that borohydride can reduce nitropropenes in high yields in the same way.
It turns out a dilemma.
Everything looks great and the video is of good quality, but judging by other sources, this cannot be.

P.S. I hope I'm wrong and it really works, because the video looks very impressive.
The reaction and it's results has been thoroughly documented and discused quite recently on thevespiary.org, which is the latest of the forums on clandestine chemistry. Check it out. Your information is outdated. This method is valid.
 
The reaction and it's results has been thoroughly documented and discused quite recently on thevespiary.org, which is the latest of the forums on clandestine chemistry. Check it out. Your information is outdated. This method is valid.

HEISENBERG+​


thanks for the replies.
indeed, it works.
(y)
 
There was a lot of controversy on this topic 20 years ago.
on the hive, on the hyperlab, on the erovid, in the literature on chemistry.
nowhere and never have I seen nitropropene reduced with sodium borohydride so easily and in high yields.
I'm not 100% sure.
but in my opinion all this is doubtful and may be a fake.
though it looks impressive.
I know that transition metal salts can be catalysts for such reductions.
but I have not seen such a reaction with such good outputs anywhere, I think if it worked, then everyone would have known about it for a long time.
in the classic formulation of rhodium, sodium borohydride can be used to reduce nitrostyrenes to phenethylamines with a normal preparative yield of the reaction product.
but never, on any site, anywhere and no one over the past 20 years has said that borohydride can reduce nitropropenes in high yields in the same way.
It turns out a dilemma.
Everything looks great and the video is of good quality, but judging by other sources, this cannot be.

P.S. I hope I'm wrong and it really works, because the video looks very impressive.
Anyone who doesn't ask how, what, why, remains stupid!!!
I've been following the whole thing online for over 20 years and from Erowid to Rhodium, Tootse or any other site that has even remotely provided such precise information about synthesis routes, procurement of raw materials and material properties!!!
 
A hose redirecting to a fume hood is mentioned, I assume for the solvent vapors, but is there also production of hydrogen gas during this reaction since NaBH4 produces it when in contact with water?

At first I assumed no since if it did, it would be a strange omission as hydrogen gas can be quite dangerous but it would be nice to have a confirmation for anyone who would like to try this.
 
A hose redirecting to a fume hood is mentioned, I assume for the solvent vapors, but is there also production of hydrogen gas during this reaction since NaBH4 produces it when in contact with water?
Looking back at the video there are small bubbles forming in the solution after the addition of the NaBH4 so I would say that there is a production of H2 gas.
 
Can copper sulfate be used instead? thats dirt cheap at the hardware store as tree stump killer... Making copper chloride isnt hard but would be annoying... same with buying it, but either way, would it work ya think?
 
the username you choose is very important on youtube.

personal I would just post a trailer on youtube and redirect people to this platform
Smart thinking man!! Didnt even think about that ,thats a good way
 
Very interesting video, I really appreciate your content! Is there any list available with all the exact equipment and chemicals that are needed?
 
is it necessary to stir for 6 hours while you add the P2NP, or do you only stir for as long as it takes to dissolve it safely?
 
I have some doubts about the chemical synthesis of amphetamine that I have seen in the video.
What percentage should the IPA , sodium borohydride, copper chloride, anhydrous acetone, sulfuric acid or orthophosphoric acid, dry cold acetone have? and they can be bought in any store or only in chemical stores?
What capacity should the Büchner flask and the separatory funnel have?
What is that metal cup that is on top of the hot plate and below the 3-headed flask?
thank you all!
 
Would be interesting to see how to lysate the salts. I know most people probably are not interested in lisdexamphetamine, as it is a prodrug, but it is a good medication that can be prohibitively expensive due to it being under patent.
 
I don't know why this video was done on such a large scale. if you do this rx for the first time, please don't do 250 g P2NP! Do something like 5 and see how it goes. It can actually be a bitch to get this one to work, even for experienced clandestine chemists. Do trial runs.

Also, why are you using acetone on a freebase amine? You'll create unnecessary imines. IPA should work just as fine.
 
Hello Community and thx for this Video, am a bit lag in english and i have a question. When i (only) have the oil are the steps in the Video the same till i get the paste? wonderin there are so much ways to get there but the on in the video seems the safest !

Greetings
 
We expect that our channel will also be deleted sooner or later, so all videos are duplicated on the forum. Download them to yourself, sooner or later they will be hard to find. I don't think anyone would be willing as we are to invest as much effort and resources in creating such a high quality video on the subject of syntheses.

True thing.

And would be nice to have the possibility to download an archived version of the entire website. HTML version, no source code.
 
THAT'S THE FINAL PRODUCT OR THERE IS MORE TO IT ? WHAT ABOUT CRYSTALLIZATION ?
 
THAT'S THE FINAL PRODUCT OR THERE IS MORE TO IT ? WHAT ABOUT CRYSTALLIZATION ?
This is gonna yield you pretty pure racemic d and l isomer amphetamine id imagine, I haven't watched the video in a while but I believe its reductive amiantion reducing p2np with NA BH4 USING the anhydride to reduce the nitropene etc etc, if you are still lost maybe a more simple compound would help, the mescaline from styrene helped me understand a bit more about the science that's going on, if this looks like too much watch the video for just the d isomer because people have lost their minds and it's a simple titration using a simple but tedious method and I've read along some of the folks on here have the synthesis down to yield the racemic product when converting the l back to d Is no where near as hard as it is to obtain FB AND PH it, then pull it, but there are simpler methods for simpler compounds that when learned will get you ready for this pretty complex reaction
 
I have been waiting for this! nice video. A couple of questions:
One of the necks on three neck flask is used for the overhead stirrer, another is used for the additions and the last one is for the thermometer and "has to be opened and directed to a fume hood" if one does not have access to a fume hood, can't one of the necks instead be used for a hose that redirects the gas elsewhere and leave the thermometer?
And to do this can't you just use a stir bar instead of the overhead stirrer? Even if you have to scale the reaction down?
I may add, if running a distillation placing the thermometer at the stillhead, then placing a glass inlet tube down into the solution and then pulling your vacuum. It will channel Everything in the direct and bring the mp/bp down as well. Yay.
 
This is gonna yield you pretty pure racemic d and l isomer amphetamine id imagine, I haven't watched the video in a while but I believe its reductive amiantion reducing p2np with NA BH4 USING the anhydride to reduce the nitropene etc etc, if you are still lost maybe a more simple compound would help, the mescaline from styrene helped me understand a bit more about the science that's going on, if this looks like too much watch the video for just the d isomer because people have lost their minds and it's a simple titration using a simple but tedious method and I've read along some of the folks on here have the synthesis down to yield the racemic product when converting the l back to d Is no where near as hard as it is to obtain FB AND PH it, then pull it, but there are simpler methods for simpler compounds that when learned will get you ready for this pretty complex reaction
THAT went over my head. i have amp salts now how do i convert to meth crystals ?
 
THAT went over my head. i have amp salts now how do i convert to meth crystals ?
You have salts as in you synthesized the amphetamine hcl? Are you trying to convert pharmaceutical amphetamine into something else, if you let me know what you have or goal is that helps me and the veteran members better assist, the freebase is synthesized then usually turned into the salt, usually by gassing it off with muriatic acid or the sulphate form by using sulphuric acid, if you're trying to clean up some dirty. Look for amphetamine salt or if you are trying to convert the l isomer into the d I could pm you the details because it's easy but easy to over complicate, go to the home page and ask G Patton for his input he will know everything you could have a question for I mean he's a true genius
 
THAT went over my head. i have amp salts now how do i convert to meth crystals ?
No I believe they don't show the finished product, they show the amphetamine salt that was created from this synthesis method, the reaction is not impossible for a noobie like myself to grasp however it's not just as easy as baking a cake, I know in the video they show it being filtered off when all the solvent is gone usually it's then left in the freezer or brought to stable weight at room temp and atmospheric pressure (not under vacuum) the next step id imagine to clean it up you could soak it in acetone overnight, the quantity would have to be scaled to the portions used, from there you filter off the acetone under vacuum as it's quicker but there's other ways they don't work as well from there you can clean again or recrystallize with methanol, super simple for the most part if you already obtained the salt from a freebase
 
Hello friends, is the final product of this video amphetamine sulfate or amphetamine base?
 
If I have amphetamine freebase in toluene how do I precipitate amphetamine sulfate, do I dilute sulfuric acid with acetone or isopropyl alcohol?
 
Amphetamine is my weakness. I hope all dealers in the UK will soon learn to make quality amphetamine.
 
I hasten to notice that there is very little relevant and up-to-date information on the Internet. Therefore speaking about other sources - they are all outdated and irrelevant. It is necessary to keep up with the times.
I also did quite a lot of unpublished work on this method but never scaled up with quite a few successes even. This procedure is pretty straight ahead and with decent results for the amount of work.
 
anyone having issues downloading the video? I am using Tor and also tried using the clear net link, every time I try to download the videos it just shows its download but no progress and then it disappear

I am using public wifi could it be the slow speed?

Thank you for all the help
 
anyone having issues downloading the video? I am using Tor and also tried using the clear net link, every time I try to download the videos it just shows its download but no progress and then it disappear

I am using public wifi could it be the slow speed?

Thank you for all the help
Right click the download link and “save link as” usually allows it to finish
 
There was a lot of controversy on this topic 20 years ago.
on the hive, on the hyperlab, on the erovid, in the literature on chemistry.
nowhere and never have I seen nitropropene reduced with sodium borohydride so easily and in high yields.
I'm not 100% sure.
but in my opinion all this is doubtful and may be a fake.
though it looks impressive.
I know that transition metal salts can be catalysts for such reductions.
but I have not seen such a reaction with such good outputs anywhere, I think if it worked, then everyone would have known about it for a long time.
in the classic formulation of rhodium, sodium borohydride can be used to reduce nitrostyrenes to phenethylamines with a normal preparative yield of the reaction product.
but never, on any site, anywhere and no one over the past 20 years has said that borohydride can reduce nitropropenes in high yields in the same way.
It turns out a dilemma.
Everything looks great and the video is of good quality, but judging by other sources, this cannot be.

P.S. I hope I'm wrong and it really works, because the video looks very impressive.
did you test it out É
 
Question.... is the temperature to be maintained below 60c for safety so it doesn't run away from you or because the actual reaction will fail if it goes over 60c?
 
Question.... is the temperature to be maintained below 60c for safety so it doesn't run away from you or because the actual reaction will fail if it goes over 60c?
there is an exothermal phenomenon that occurs with some induction time so adding copper solution should be executed steadily and with pauses
 
Okay I am having an issue with this reaction. Everything is used exactly like in the video every the substance. The timing of everything I kept with in the constraints of the instructions and the p2np is perfectly clean and re-crystallized immediately before with nice long light yellow needles. The first time I did the reaction it worked. Every time since I get a very very bright white substance that almost smells a little fruity. Different than the first time which had a slightly tan color to it. I made much smaller batches just for personal and was all calculated down properly. What is this bright white substance I am getting at the end which I am much more afraid to try than the first one lol?
 
I've done this reaction in ethanol as a solvent, and the yeild is better comparing to IPA.
I've used 60/40 ETOH/H2O to dissolve NaBH4.
Reaction in ethanol is faster and I've obtained much cleaner product.
Also is good rule of thumb to acidify the RM after the reduction, and wash it with petroleum ether to clean some side products and unreacted P2NP. It can be seen in this video as yellow color after basification.
To extract freebase I've also used petroleum ether, and used IPA to dissolve H2SO4.
This is cheap way for extract every freebase that I work with.
Don't use acetone to mix with H2SO4, because it will react and form dark solution.
Good luck for everyone entering the clandestine world :)
 
are all of these compounds directly scalable to different sized reactions? Someone (maybe the poster) typed up a way scaled down version and all the ratios are different....

also if CuSO4 can be substituted for CuCl2, can you use the same amount, or do you have to calculate for the same amount of copper by weight in the substitution?
 
I've done this reaction in ethanol as a solvent, and the yeild is better comparing to IPA.
I've used 60/40 ETOH/H2O to dissolve NaBH4.
Reaction in ethanol is faster and I've obtained much cleaner product.
Also is good rule of thumb to acidify the RM after the reduction, and wash it with petroleum ether to clean some side products and unreacted P2NP. It can be seen in this video as yellow color after basification.
To extract freebase I've also used petroleum ether, and used IPA to dissolve H2SO4.
This is cheap way for extract every freebase that I work with.
Don't use acetone to mix with H2SO4, because it will react and form dark solution.
Good luck for everyone entering the clandestine world :)
can u create a step by step post for ur synthesis....
 
This was really useful to see the workup performed in front of my eyes….

I’m not really planning on doing this with much P2NP BUT I do have various substituted nitrostyrene’s and nitropropene’s that I DO need to reduce….

I tried it once but I don’t think I actually added enough CuCl2 as i don’t think It went black but I think the main thing was I fucked up the workup….

I even got so pissed off I decided to try the Zn/HCl method

Anyway, thanks for this video
 
Wouldnt it be usefull to add KOH to the solution before adding NaBH4 ? To reduce the degradation rate ?
Maybe cooling in an ice bath while adding p2np, keeping as low as possible ? After that letting it stir for longer
And drying the freebase ipa solutions before precipitating.
60% yield is quite low
 
Wouldnt it be usefull to add KOH to the solution before adding NaBH4 ? To reduce the degradation rate ?
Maybe cooling in an ice bath while adding p2np, keeping as low as possible ? After that letting it stir for longer
And drying the freebase ipa solutions before precipitating.
60% yield is quite low
I have been performing this reaction using a bunch of different conditions and found that after adding cucl2 which I add slowly dripping so it converted to free cu(0) as fine particles without the copper grouping together then having to wait for it to reduce to fine particles and use a lesser amount of nabh4 and still find the reaction completing without even heating at all. I let the solution completely come down to room remp before adding cucl2 and allow it to heat on it own which hits around 50c usually and by the time the copper naturally settles to the bottom it's completely done. Every single time I try to follow the videos directions exactly I end up going past the amine group and end up completely over reducing it. I started dissolving p2np in alcohol and water pretty much the same as used in the video as in amounts and then adding nabh4 in small amounts allowing 15 minutes at least in between additions and once I get a clear solution or clear white ish I have been adding say another gram of nabh4 per 5 G of p2np at that point allowing it to stir and slowly adding in the Catalyst then I can get to 30 minutes of heating at 80c to finish. If I use 7.5 eq of nabh4 i blow right past it every time watching the amine quickly form at near room temp and dwindle away to almost nothing at the end of 30 minutes at 80c.
 
I have been performing this reaction using a bunch of different conditions and found that after adding cucl2 which I add slowly dripping so it converted to free cu(0) as fine particles without the copper grouping together then having to wait for it to reduce to fine particles and use a lesser amount of nabh4 and still find the reaction completing without even heating at all. I let the solution completely come down to room remp before adding cucl2 and allow it to heat on it own which hits around 50c usually and by the time the copper naturally settles to the bottom it's completely done. Every single time I try to follow the videos directions exactly I end up going past the amine group and end up completely over reducing it. I started dissolving p2np in alcohol and water pretty much the same as used in the video as in amounts and then adding nabh4 in small amounts allowing 15 minutes at least in between additions and once I get a clear solution or clear white ish I have been adding say another gram of nabh4 per 5 G of p2np at that point allowing it to stir and slowly adding in the Catalyst then I can get to 30 minutes of heating at 80c to finish. If I use 7.5 eq of nabh4 i blow right past it every time watching the amine quickly form at near room temp and dwindle away to almost nothing at the end of 30 minutes at 80c.
If it gets over cooked does it mess up the yield ? Is the product still usable or is it poisonous ? I am hoping to get a grip on this copper synth and the amalgam synth and then move on to new synths after
 
So is that the correct ratio of copper chloride or is it just keep adding copper chloride until it stops putting out black sediment ?
 
I tried this synth and the yield was next to nothing. Can someone do a good write up of a 5g reactions. I did 8.5g boro, 100ml ipa, mix for 30min, add p2np 2g over a time of 60min, let mix for additional 30 min, add copper dropwise .5g over time of 90minutes, react for further 3hrs on 120 Fahrenheit. Pour off liquid, basify, pull of ipa, acidify, I got .25 back maybe and idk if it correct product or not?

is the product supposed to be able to be smoked as freebase ? Because this product just turns to black ash
 
I tried this synth and the yield was next to nothing. Can someone do a good write up of a 5g reactions. I did 8.5g boro, 100ml ipa, mix for 30min, add p2np 2g over a time of 60min, let mix for additional 30 min, add copper dropwise .5g over time of 90minutes, react for further 3hrs on 120 Fahrenheit. Pour off liquid, basify, pull of ipa, acidify, I got .25 back maybe and idk if it correct product or not?

is the product supposed to be able to be smoked as freebase ? Because this product just turns to black ash
Just like the video you yes add the copper drop wise but like a drop about every second... definitely not 90 minutes. And 120c where did you see that temperature? 80c and for only 30 minutes that's it... 70c would easily do it. Hell they reduce nitro groups in minutes at room temperature. Where did you get those instructions. You can go overboard. More is not more in this case.
 
I usually just squeeze it in with a syringe all at once 🤷‍♂️
Works fine…
Iv used this synthesis on like 4 different nitroalkene’s now so it definitely works and I got like a 73% yield when I last did it so the synthesis works for sure!
I wouldn’t personally bother doing it in less than like a 10g reaction though tbh I was trying to do 5g reactions at first and was fecking it up or getting hardly anything in return so I scaled up (so at least I would obtain something) and then repeated lots to improve my yields and figure out what was going wrong (it was purity of reagents)

Maybe try that? I dunno
 
I’m actually about to do it again but with md-p2np and I have no doubt it will work okay.
I do want to learn how to do an Al/Hg amalgam though - get cheap cheap foil to do the heavy lifting lol
 
I would give a couple of pointers on this reaction actually.
Firslty just listen to the OP’s advice and purify purify purify your inputs.
Secondly, if when you basify and separate layers, the organic layer is a nasty colour other than amber, just wash it with more base. Sounds stupid to say because it’s a stupidly simple thing, but i kept getting these nasty coloured layers at first.
Thirdly, after you have added the nitroalkene, just let it react under ice until you see no more colour. Sometimes it takes ages (I can’t remember specifically with p2np if it does take ages but certainly other nitroalkene’s can take ages) just let it go on ice until it’s white, it will eventually go white - then add you catalyst.

I just dump the catalyst, dissolved in a little water, into the mix while it’s cold and use the exotherm to start warming everything up. Dunno if that’s how it’s meant to be done - probably not, but hey! It works!
 
So is that the correct ratio of copper chloride or is it just keep adding copper chloride until it stops putting out black sediment ?
Well that's kind of tricky to answer because it depends on the quality of your p2np and how long you are reacting the total mixture before putting in the copper. Over time the nabh4 will be less and less and less. Based on the original amounts in the video Once you adjust it to how much you're using it sounds like if it has reacted for as much time as the video then half of it would do the job. I find it kind of hard to tell in the first place because the whole flask turns black. Most people just dump it in in the first place. Sounds like it works both ways. If you start adding copper and you see the reaction temperature climbing the copper is being reduced and all is good. Once the temperature stops rising and stalls put it on heat and continue the rise to 80° C. I usually start the 30 minute timer as the reaction crosses 60° C because the Nitro group is reduced pretty quickly and would most likely happen at room temperature to begin with in minutes.
 
Yeah I would agree with all of that. I personally just use a standard catalytic amount 1-5% typically.
Yeah I do a similar thing with regards adding it.
I do it like this…
Add the iso/water, put in ice bath, chuck in the borohydride in one. Or sometimes I split it into two and add the second half later. Then slowly add the nitroalkene over an hour (I always do a 10g reaction) but obviously if you do a 5g add it over 1/2h, then I just leave it for a few hours checking it every so often to replace ice etc until a point when the colour has completely disappeared and it’s gone white, remove ice bath, switch to a larger flask, add the catalyst in water in one go from a pipette - someone said try not to let it have air contact so I just stick the pipette near the RM and add it all in one go, use the exotherm to raise the temp to 60c for half an hour, then I raise it to 80c for half an hour also. Honestly the 60c half hour usually goes up to around 70c and has been fine.
I know most people don’t do both half an hour at 60 then again at 80. You maybe don’t need to, iv just noticed it takes a while under reflux before layers start separating. You are PROBABLY okay once this happens but I dunno coz iv never tried.

I don’t tend to do this reaction with p2np tbh, I tend to be reducing other nitroalkene’s but it’s all the same (with adjusted mol equivalents, of course)
When I did it with 10g of 3,4,5-TMONS I ended up with a return of 8g…great yield.

Then I did it again with 9g md-p2np and ended up with 6.7g return - which I calculated to 77.9% yield. V happy and comfortable with this method of reducing things now…

I still do want to try the Al/Hg amalgam method though. Seems cheaper to rely on foil but obviously the trade off is that you have to dispose of mercury waste 🤷‍♂️

My advice is to just keep trying if you get a crap yield because I also got a crap yield at first - I believe because I wasn’t allowing it long enough to reduce to the colourless intermediate before adding the catalyst.

Just read up and try people’s advice basically.
 
Al\Hg is far superior regarding quality of product when regarding amphetamine at least and the actual drawback consists of the maximal scale the Hg waste is not that much of a problem since you can't make that much. NaBH4/CuCl2 is suitable for larger quantities but amp always has an undesirable characteristic aroma.
 
Al\Hg is far superior regarding quality of product when regarding amphetamine at least and the actual drawback consists of the maximal scale the Hg waste is not that much of a problem since you can't make that much. NaBH4/CuCl2 is suitable for larger quantities but amp always has an undesirable characteristic aroma.
That’s interesting.
I don’t do amphetamine so I’m inexperienced with it
why no alkaline on second pull of solvent?
Do you mean when you wash the aqueous phase with more IPA? You don’t need to re-basify because the base is already sat there, from when you removed the first lot.
From my understanding here, you basify it so that all the amine is freebased and pulled into the organic phase and to promote phase separation. Once that has happened, it’s happened and doesn’t need repeating.
I would say unless your organic phase looks dirty there is no point re-basifying. It does do wonders to pull out any copper remaining though so yeah if it’s dirty then you can wash it with a base.

I may have misunderstood your question though…
 

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