One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[WillD]

Is normal to have a solid precipitate after point 6? I made twice with the same result I just filtered.

btcboss2022Yes, an insoluble precipitate should fall out. So, we remove excess salts, getting the base.

 

[syntheticdrugs]

Yes, an insoluble precipitate should fall out. So, we remove excess salts, getting the base.

William Dampier

William DampierHello, can I use something else instead of sodium borohydride in this reaction?​

 

[G.Patton]

William DampierHello, can I use something else instead of sodium borohydride in this reaction?​

syntheticdrugsHello, yes. Al/Hg, LAH, Pd/C and H2, Ni/Re and H2. Last two are quite not recommended for a novice.

 

[Mr.Magic]

Hi, I'm fairly new to organic chemistry (9 month or so now, no other experience in chemistry )and have synthesized amphetamine via the Al/Hg route a few dozen times in the last couple of months.

I was able to reduce up to 120g of P2NP in a 20L round bottom flask. The purity of the end product was phenomenal in the last syntheses.
Most of the time I only had to purify the amphetamine sulfate once pro forma with acetone because it was already so white.

I found the NaBH4/CuCl²-route interesting because I have a great deal of respect for working with mercury, it had already led to a violent exothermic reaction three times, a large amount was distributed throughout the room and I would like to do without it in future.

The reduction with NaBH4/CuCl² also allows a significantly higher yield with a flask that is only half the size.
So far I have synthesized three times. The first time 80g P2NP, the second time 200g P2NP and the last time 250g P2NP.
The last one was the best of all, as I managed to stick exactly to the temperatures.

What I should also mention is that in order to shorten the process of administering P2NP, I place the flask in a large container full of ice, which I then heat over a hotplate. I was able to fill the entire 250g of P2NP into the flask in a good three quarters of an hour without getting above the 60°C mark. Does this affect the reaction with the Borohydride?

Despite all the care taken, the sulfate has a somewhat sweet, pungent smell at the end, despite its snow-white color. The consistency is also much more crystalline, crunching softly when crushed.
I have cleaned it several times with acetone and DCM, filtered it in a Buchner funnel, etc.
It definitely seems that another salt has joined the sulfate.

Has something similar ever happened to you?

Is it possible that the Sodium Borohydride, if not completely dissolved, mixes with the amphetamine freebase and is converted to a sodium salt when neutralized with H²SO4?
The stuff also burns badly in the nose. A friend had watery nasal mucus running out of his nose for several minutes immediately after taking a drag.

And now the real question: if there is another salt in it, how or what method can I use to separate the two substances?
I'm slowly coming to the end of my tether.

Thank you in advance for your patience in reading the whole text

I am grateful for any advice.

Mr.Magic

 

[OrgUnikum]

Hi, I'm fairly new to organic chemistry (9 month or so now, no other experience in chemistry )and have synthesized amphetamine via the Al/Hg route a few dozen times in the last couple of months.

I was able to reduce up to 120g of P2NP in a 20L round bottom flask. The purity of the end product was phenomenal in the last syntheses.
Most of the time I only had to purify the amphetamine sulfate once pro forma with acetone because it was already so white.

I found the NaBH4/CuCl²-route interesting because I have a great deal of respect for working with mercury, it had already led to a violent exothermic reaction three times, a large amount was distributed throughout the room and I would like to do without it in future.

The reduction with NaBH4/CuCl² also allows a significantly higher yield with a flask that is only half the size.
So far I have synthesized three times. The first time 80g P2NP, the second time 200g P2NP and the last time 250g P2NP.
The last one was the best of all, as I managed to stick exactly to the temperatures.

What I should also mention is that in order to shorten the process of administering P2NP, I place the flask in a large container full of ice, which I then heat over a hotplate. I was able to fill the entire 250g of P2NP into the flask in a good three quarters of an hour without getting above the 60°C mark. Does this affect the reaction with the Borohydride?

Despite all the care taken, the sulfate has a somewhat sweet, pungent smell at the end, despite its snow-white color. The consistency is also much more crystalline, crunching softly when crushed.
I have cleaned it several times with acetone and DCM, filtered it in a Buchner funnel, etc.
It definitely seems that another salt has joined the sulfate.

Has something similar ever happened to you?

Is it possible that the Sodium Borohydride, if not completely dissolved, mixes with the amphetamine freebase and is converted to a sodium salt when neutralized with H²SO4?
The stuff also burns badly in the nose. A friend had watery nasal mucus running out of his nose for several minutes immediately after taking a drag.

And now the real question: if there is another salt in it, how or what method can I use to separate the two substances?
I'm slowly coming to the end of my tether.

Thank you in advance for your patience in reading the whole text

I am grateful for any advice.

Mr.Magic

Mr.MagicAmmonium sulfate or sodium sulfate contamination, I would for the burning guess ammonium sulfate. You have to dissolve the Amph-base in an solvent like Toluene or Xylene and then wash it with water to remove the ammonia. As Ammonia is very very water soluble but Amph base is almost not at all so if you are generous with the Xylene like 5 times the amount of base, you can wash out the ammonia with two washes water of the same amount as the base is. Completely and without losses.
Also steamdistillation of the base is needed to get rid of the dimeric byproduct.

Rolled into one, steamdistill the base directly from the flask, it will come over easily and completely then add Xylene 5 time the amount of the oil, separate the two layers and add water (as much as the oil was) shake and wait, separate and now you have Amph base fre from Ammonia, any sodium and the byproduct from step one.

 

[WillD]

Washing with water after the first stage and extraction in general is desirable to obtain a pure product without any burning.

 

[mithyl2]

Washing with water after the first stage and extraction in general is desirable to obtain a pure product without any burning.

William Dampieris this as simple as adding water after all of the boro and p2np has been added, and then continuing with the synthesis as normal?

could you elaborate a little?

 

[mithyl2]

Carefully dilute the reaction with water, extract an intermediate product from the mixture using ethylacetate (as an example) for use in the next reaction.

William DampierApologies if I'm being stupid and I don't want to be annonying with too many noob questions, but do you mean extracting the amphetamine with ethylacetate from the ipa mixture that has just been seperated from the black copper oxide?

 

[OrgUnikum]

Some theoretical background: P2NP is a so called Nitroalkene what means there s a double bond in the molecule. To get this to the Amine first this double bond is reduced forming a Nitroalkane. The Nitroalkane is reduced to the Amine by NaBH4/Cu(II) without issues. The problem is in the first reduction of this double bond as there is a competing reaction taking place (I spare you the details, its a "Michaels addition"). To solve the problem (partly) a huge amount of NaBH4 is used and the reaction runs hot and fast, it is a race: The faster one gets to the Alkane the less side-reaction. Nevertheless the side reaction cannot be completely eliminated this way. Also the huge amount of NaBH4 needed is wasteful, the reaction volume is huge too, runaways are possible.... Better then the acidic Al/Hg but far from perfect.

After quite some reading up on this I think I know a way to solve some of this. I would try it myself, but I have no P2NP at the moment and I do not want to buy something like this just now for other reasons. Well I tell how I would try this:

60 g NaBH4 and 500 g silica gel or diatomeous earth (chromatography quality) and 200 ml DCM are mixed thoroughly using a kitchen-dough kneader and put in a 3 liter flask.with overhead stirrer. IPA is added to make a stirable slurry and then P2NP 100 g in IPA is dripped in keeping the temperature at 25°C or below. Coo so needed.

There are plenty od wxamples for this reaction scheme and it is used to prevent exactly this kind of side reaction from happening. The unwanted reaction is caused mostly due to the ph of the reaction being to alkaline. The silica-gel being acidic lets the reaction take place on the surface of the gel and there ph is about 3 although the solvent is much more alkaline.

After all the P2NP was added the reaction is stirred (as slurry) until the yellow color of P2NP is completely gone. (if it does not go, add some more NaBH4, no problem)

Then more IPA is added, the CuCl2, 6 g, and 30 g more NaBH4 and the rest is the same as known.

Advantages are obvious, I bet with some optimizing NaBH4 and volume of reaction can be reduced further. It will work the better the better the NaBH4 is impregnated onto the the silica gel.

I would recommend to always steamdistill or vacuum distill the amphetamine base from any NaBH4 reduction of P2NP (same if using Al/Hg) as otherwise there will be some contamination by unpleasant dimeric products, the side reaction can be reduced but its nigh to impossible to get rid of it (using NaBH4 at least).

I read here that copper oxide is precipitating as black powder. This seems to me a bit strange, why should this happen in presence of a strong reducing agent? I say thats metallic copper nano-particles, the salt reduced to the metal, those particles do the actual reducing job, nitro-alkane to amine utilizing hydrogen supplied by NaBH4. But I might be wrong here, I did not look so closely into this part as it is not the problem.

If somebody would try this, would be great, or somebody in the EU donate me some P2NP and I try it myself and post the results.

 

[zeus]

Some theoretical background: P2NP is a so called Nitroalkene what means there s a double bond in the molecule. To get this to the Amine first this double bond is reduced forming a Nitroalkane. The Nitroalkane is reduced to the Amine by NaBH4/Cu(II) without issues. The problem is in the first reduction of this double bond as there is a competing reaction taking place (I spare you the details, its a "Michaels addition"). To solve the problem (partly) a huge amount of NaBH4 is used and the reaction runs hot and fast, it is a race: The faster one gets to the Alkane the less side-reaction. Nevertheless the side reaction cannot be completely eliminated this way. Also the huge amount of NaBH4 needed is wasteful, the reaction volume is huge too, runaways are possible.... Better then the acidic Al/Hg but far from perfect.

After quite some reading up on this I think I know a way to solve some of this. I would try it myself, but I have no P2NP at the moment and I do not want to buy something like this just now for other reasons. Well I tell how I would try this:

60 g NaBH4 and 500 g silica gel or diatomeous earth (chromatography quality) and 200 ml DCM are mixed thoroughly using a kitchen-dough kneader and put in a 3 liter flask.with overhead stirrer. IPA is added to make a stirable slurry and then P2NP 100 g in IPA is dripped in keeping the temperature at 25°C or below. Coo so needed.

There are plenty od wxamples for this reaction scheme and it is used to prevent exactly this kind of side reaction from happening. The unwanted reaction is caused mostly due to the ph of the reaction being to alkaline. The silica-gel being acidic lets the reaction take place on the surface of the gel and there ph is about 3 although the solvent is much more alkaline.

After all the P2NP was added the reaction is stirred (as slurry) until the yellow color of P2NP is completely gone. (if it does not go, add some more NaBH4, no problem)

Then more IPA is added, the CuCl2, 6 g, and 30 g more NaBH4 and the rest is the same as known.

Advantages are obvious, I bet with some optimizing NaBH4 and volume of reaction can be reduced further. It will work the better the better the NaBH4 is impregnated onto the the silica gel.

I would recommend to always steamdistill or vacuum distill the amphetamine base from any NaBH4 reduction of P2NP (same if using Al/Hg) as otherwise there will be some contamination by unpleasant dimeric products, the side reaction can be reduced but its nigh to impossible to get rid of it (using NaBH4 at least).

I read here that copper oxide is precipitating as black powder. This seems to me a bit strange, why should this happen in presence of a strong reducing agent? I say thats metallic copper nano-particles, the salt reduced to the metal, those particles do the actual reducing job, nitro-alkane to amine utilizing hydrogen supplied by NaBH4. But I might be wrong here, I did not look so closely into this part as it is not the problem.

If somebody would try this, would be great, or somebody in the EU donate me some P2NP and I try it myself and post the results.

OrgUnikumI can give you 50g if you can't get it. I will try this method when have the possibility and will share the results here.

 

[OrgUnikum]

Ammonium sulfate or sodium sulfate contamination, I would for the burning guess ammonium sulfate. You have to dissolve the Amph-base in an solvent like Toluene or Xylene and then wash it with water to remove the ammonia. As Ammonia is very very water soluble but Amph base is almost not at all so if you are generous with the Xylene like 5 times the amount of base, you can wash out the ammonia with two washes water of the same amount as the base is. Completely and without losses.
Also steamdistillation of the base is needed to get rid of the dimeric byproduct.

Rolled into one, steamdistill the base directly from the flask, it will come over easily and completely then add Xylene 5 time the amount of the oil, separate the two layers and add water (as much as the oil was) shake and wait, separate and now you have Amph base fre from Ammonia, any sodium and the byproduct from step one.

 

[mithyl2]

Ammonium sulfate or sodium sulfate contamination, I would for the burning guess ammonium sulfate. You have to dissolve the Amph-base in an solvent like Toluene or Xylene and then wash it with water to remove the ammonia. As Ammonia is very very water soluble but Amph base is almost not at all so if you are generous with the Xylene like 5 times the amount of base, you can wash out the ammonia with two washes water of the same amount as the base is. Completely and without losses.
Also steamdistillation of the base is needed to get rid of the dimeric byproduct.

Rolled into one, steamdistill the base directly from the flask, it will come over easily and completely then add Xylene 5 time the amount of the oil, separate the two layers and add water (as much as the oil was) shake and wait, separate and now you have Amph base fre from Ammonia, any sodium and the byproduct from step one.

OrgUnikumI appear to have successfully synthesized more amphetamine which doesn't appear to be contaminated like my previous batches and ended up with a very white and soft powder, which unfortunately smells strongly of the reaction mixture. So I'm looking to use steam distillation to purify it and then perform an a/b extraction.

when steam distilling, do i simply charge a boiling flask with water and the amphetamine solution, (after the part where i've added the naoh) and carry out the steam distillation at this point?
Also how will I know when all of the amphetamine has finished coming over?

 

[OrgUnikum]

I appear to have successfully synthesized more amphetamine which doesn't appear to be contaminated like my previous batches and ended up with a very white and soft powder, which unfortunately smells strongly of the reaction mixture. So I'm looking to use steam distillation to purify it and then perform an a/b extraction.

when steam distilling, do i simply charge a boiling flask with water and the amphetamine solution, (after the part where i've added the naoh) and carry out the steam distillation at this point?
Also how will I know when all of the amphetamine has finished coming over?

mithyl2You need a big enough flask from the beginning and when the reaction is over you add diluted ice-cold HCl or Acetic Acid (strong vinegar 20%) until ph is acidic (< 5) and then start distilling off the alcohol. You should place a thermometer at the inlet of the condenser, you know a Claisen-adapter? Thats what the second small grounded joint is for, a thermometer adapter and a thermometer going in taking the steam-temperature. Do not heat like mad but good enough to get the alcohol out like quick dip, dip dip.
When the alcohol is gone, whats when the thermometer goes over 85 °C. Let the flask cool down (or use a cold water bath or such for quick and add ice-cold !0% NaOH and more water to fill the flask to half (if you do not use a stirrer here) or two-thirds with stirrer. The cheap Chinese Stirrer bearings which are actually just thermometer adapters which have just one o-ring are not suited for steamdistillation, you will lose a lot of product escaping through this ring, trust me. So ether magnet here or no stirrer. If no stirrer a splash-head is a good thing to have, but one can do without if one is careful.
Amphetamine comes over with water at 92 ° to 96 °C. There must be always plenty water in the flask, sometimes one has to refill once or twice. Refill with almost boiling water and you lose no time at all.
What comes over at 96 °C and more up to 99 °C still has some Amph but its usually contaminated. This should be collected separately and a full A/B done for this, then it will be just fine. With some routine you will get everything at 92 °C to 96 °C but it needs some practice. If there is still IPA in the flask some A will come with the IPA at 84 °C+, so better make sure all is gone as long the soup is still acidic.
Amphetamine steams easily and so it takes not overly long to steam even bigger amounts, for big batches its not more heast but a vessel with abigger opening and a bigger (wider) condesner is what speeds things up massivly. So a 5 liter flask should have a NS45 joint and a NS45 Claisen and an intensiv cooler (coil and jacket) NS45 or NS 29 of minimum 40 cm effective length (thats without the joints) and then you have the water running out as a small stream with the oil on top of it, just charming.

Oh, and the boiling flask has to be completely insulated up to the the distillation adapter to prevent back-condensation in the flask itself. Don't be too unpatient, it takes some time until the whole thing is up to temperature and it runs properly, for those with too much money: Heating mantles for the top of flasks exist (expensive) or can be made from cheap AliExpress heating mantles and also cheap Temp controllers (PID controller).

I suppose I will make a steam-distillation tutorial with pictures if I find the time and energy for it.

 

[mithyl2]

Ammonium sulfate or sodium sulfate contamination, I would for the burning guess ammonium sulfate. You have to dissolve the Amph-base in an solvent like Toluene or Xylene and then wash it with water to remove the ammonia. As Ammonia is very very water soluble but Amph base is almost not at all so if you are generous with the Xylene like 5 times the amount of base, you can wash out the ammonia with two washes water of the same amount as the base is. Completely and without losses.
Also steamdistillation of the base is needed to get rid of the dimeric byproduct.

Rolled into one, steamdistill the base directly from the flask, it will come over easily and completely then add Xylene 5 time the amount of the oil, separate the two layers and add water (as much as the oil was) shake and wait, separate and now you have Amph base fre from Ammonia, any sodium and the byproduct from step one.

OrgUnikumafter the steam distillation, will i be able to precipitate the amphetamine from the water by adding dry acetone, and then sulfuric acid as normal? or will the amphetamine free base need to be in a solvent like ipa as per the video?
in other words, how will i precipitate the amphetamine after steam distillation in reference to what you said above?

thank you for any help.

 

[OrgUnikum]

after the steam distillation, will i be able to precipitate the amphetamine from the water by adding dry acetone, and then sulfuric acid as normal? or will the amphetamine free base need to be in a solvent like ipa as per the video?
in other words, how will i precipitate the amphetamine after steam distillation in reference to what you said above?

thank you for any help.

mithyl2I usually just add diluted H2SO4 until ph 7 and then I wash the Amphetamine Sulfate which is dissolved in water with nonpolar solvents, First ethyl-acetate and then Naphta 80/100 (Waschbenzin) to remove any organic crap which came through the steaming. Then I boil off most of the water until it gets so thick that it starts splattering, add IPA and boil this off (reduced heat) until its a white mush and flood it with Acetone and into the fridge it goes. An hour later I vacuum filter it, wash it in the filter with more Acetone and then with Naphta 40/60 (Wundbenzin) and let it dry what takes just a few minutes.
But you can also extract after steaming with any nonpolar like ethyl-acetate, toluene. xylene (Naphta is not good here) and precipitate with H2SO4 in IPA. If you add brine (concentrated salt solution) to the water you need only one extraction. Or you just add a lot of salt to the water and stir until its dissolved. If you do it this way you best add the non-polar and salt to the receiving flask and put it on a magnet stirrer then it is only separate (dry if you feel like it) and add H2SO4 in IPA and you are there. I strongly recommend to wash the final product with Acetone and then with Naphta 40/60, it very much improves the quality.

 

[mithyl2]

I usually just add diluted H2SO4 until ph 7 and then I wash the Amphetamine Sulfate which is dissolved in water with nonpolar solvents, First ethyl-acetate and then Naphta 80/100 (Waschbenzin) to remove any organic crap which came through the steaming. Then I boil off most of the water until it gets so thick that it starts splattering, add IPA and boil this off (reduced heat) until its a white mush and flood it with Acetone and into the fridge it goes. An hour later I vacuum filter it, wash it in the filter with more Acetone and then with Naphta 40/60 (Wundbenzin) and let it dry what takes just a few minutes.
But you can also extract after steaming with any nonpolar like ethyl-acetate, toluene. xylene (Naphta is not good here) and precipitate with H2SO4 in IPA. If you add brine (concentrated salt solution) to the water you need only one extraction. Or you just add a lot of salt to the water and stir until its dissolved. If you do it this way you best add the non-polar and salt to the receiving flask and put it on a magnet stirrer then it is only separate (dry if you feel like it) and add H2SO4 in IPA and you are there. I strongly recommend to wash the final product with Acetone and then with Naphta 40/60, it very much improves the quality.

OrgUnikumthank you so much for all of this info. am working through it and will put it to good use very soon.

is 45% orthophosphoric acid ok to use when precipitating the amphetamine salt?

 

[41Dxflatline]

You can catalyse this reaction with powdered human hair instead of copper salts

 

[mithyl2]

You can catalyse this reaction with powdered human hair instead of copper salts

41DxflatlineAre you serious?

Is this what you are talking about:

https://www.researchgate.net/publication/339852077_Human_Hair_Catalyzed_Selective_Reduction_of_Nitroarenes_to_Amines

 

[mithyl2]

i've performed a couple A/B extractions, but the oil layer that forms on the top of the dissolved amphetamine in water after i add the naoh is so thin it's hardly there. this has happened with all of the batches of amphetamine i've made, which probably means that the amphetamine i'm working with actually doesn't contain much amphetamine at all.
this seems consistent with the reagent tests i did where when i tested the amphetamine before A/B extraction it did test positive, but the marquis reagent was only a faint brown red that comes slowly. but when i tested this same amphetamine after it had been through an A/B extraction it immediately turned a strong brown/red color.
the problem is that the amount of this pure amphetamine i got was an unbelievably appalling 0.22% yield (5g un-purified amphetamine, and after the A/B i got 0.011mg amphetamine.

what could be the reason for this?

 

[TheCook]

i've performed a couple A/B extractions, but the oil layer that forms on the top of the dissolved amphetamine in water after i add the naoh is so thin it's hardly there. this has happened with all of the batches of amphetamine i've made, which probably means that the amphetamine i'm working with actually doesn't contain much amphetamine at all.
this seems consistent with the reagent tests i did where when i tested the amphetamine before A/B extraction it did test positive, but the marquis reagent was only a faint brown red that comes slowly. but when i tested this same amphetamine after it had been through an A/B extraction it immediately turned a strong brown/red color.
the problem is that the amount of this pure amphetamine i got was an unbelievably appalling 0.22% yield (5g un-purified amphetamine, and after the A/B i got 0.011mg amphetamine.

what could be the reason for this?

mithyl2It would help if you describe exactly how you proceeded, what purity your reagents have, how large your batch was, etc...

 

[mithyl2]

It would help if you describe exactly how you proceeded, what purity your reagents have, how large your batch was, etc...

TheCookthe A/B extractions i'm referencing here are from 2 different batches. one with 20g p2np and the other with 15g. neither used recrystallized p2np because it appeared to be of a high enough quality to use as it and also a genuine product as determined by mp. (however i've already recrystallized a batch ready for my next synthesis in case it isn't.)

i dried my acetone with mgso4 with it sitting in the acetone for around 24 hours before i filtered it.

all my proportions were the same as in the corresponding tutorial video, i used 'CuSO4*5H2O' which should work fine.

all of my reagents are lab grade. as far as the method is concerned i followed the procedures as what was done in the video, but there are a few exceptions:

i did have a bit of trouble with adding the CuSO4*5H2O. for both batches i added it slowly in a few drops, then turned on the heat, then proceeded to slowly add the rest dropwise. for the 20g batch the heat was fluctuating between 78c-83c because of my shit heating mantle, but this didn't happen with the 15g batch as it remained at 80c, but it stayed there for maybe 40-70 minutes.
also, for the 20g batch i left the solution sitting in the flask with the copper sludge at the bottom for a couple of days before decanting it. i didn't do this with the 15g batch as i decanted it straight away.

i didn't use 98% pure acid when it came to precipitation at the end, instead it was diluted with 55% water. perhaps this is the problem?

i had this same problem for the A/B extraction with both batches, the problem being that both batches only had a tiny oil layer which contains the amphetamine form at the top of the solution after i added the naoh when it should have been far more.

 

[OrgUnikum]

I do not know why everybody seems to think making the sulfate by adding concentrated H2SO4 to AMph base in Acetone is a good idea. AFAIK even in the scientific articles they had at best 70% yield, say they lost 30% of the produced Amphetamine by making the salt whats just ridiculous. I meanwhile believe somewhere there is a chemists grave and one can hear neverending laughing from the chemist who wrote this crap to fool youngsters who want to make speed.
Look Acetone and concentrated H2SO4, thats already not so good an idea, hitting something rather sensible like an primary Amine with a strong and oxidizing mineral acid without any water around, well thats also not really convincing. It is such an unnecessary waste, why not treat the Amph nicely, be gentle, I mean it brings you joy and money.... so why mistreat it?

 

[mithyl2]

what is the best way to distill off the IPA after the addition of the CuSO4*5H2O and heating at 80C for 30 minutes, so that only IPA comes over and none of the H2O? I have a couple of ideas but need some advice.

 

[mithyl2]

when i tried fractional distillation i think some of the water came through with the ipa. and the heat was only at 80c the entire time of the distillation. i've done this a couple of times before where if i leave the distillation going i'll just end up with the copper as a solid goo, and no liquid.
i'll precipitate the amphetamine asap and see what the product is like, as maybe the ipa was present as a contaminant in previous batches.

are there any suggestions on what i can do to make sure i get only the ipa, and none of the water containing amphetamine?

i'll be trying variations of this synthesis as well.

 

[OrgUnikum]

when i tried fractional distillation i think some of the water came through with the ipa. and the heat was only at 80c the entire time of the distillation. i've done this a couple of times before where if i leave the distillation going i'll just end up with the copper as a solid goo, and no liquid.
i'll precipitate the amphetamine asap and see what the product is like, as maybe the ipa was present as a contaminant in previous batches.

are there any suggestions on what i can do to make sure i get only the ipa, and none of the water containing amphetamine?

i'll be trying variations of this synthesis as well.

mithyl2IPA forms an azeotrope with water so all IPA you distill will have about 30% water in it. You can distill the IPA off without the possibility to have some amphetamine coming over either by vacuum distillation, only a little vacuum like an aspirator pump produces is sufficient, say, when you have have the IPA coming at 60 °C or less there will be no amphetamine in it. Or you render the reaction acidic by adding diluted acetic acid until ph is 3 or less. The amphetamine will form a salt and not distill. Let cool down, then add ice-cold 10% NaOH solution until ph 12 and steamdistill the Amphetamine base.

It must be told, that the addition of 20% NaOH "to basify the reaction" is completely bs as if you measure it you will find the reaction is already alkaline like hell, ph 12 or more as the NaBH4 and its products are all strong bases. Why it is in the original text I cannot fathom, why it was posted here, well.... This happens if you lift something from an article or here thesis 1 to 1 without really knowing or trying. See attached document page 20 and page 30, on page 30 you will find the procedure word by word.
The problem is obvious: You have a mixture of water and IPA and Amphetamine. You could add brine and so salt the IPA with the Amph out, that would work well. But adding NaOH 20% will not suffice to salt the IPA out but in the best case some Amph will come to the top and this will contain IPA. Or you extract IPA and Amph with a water insoluble nonpolar solvent. This works also well. Or do as described above. In any case, check the ph and you will find that NaOH to make it more basic/alkaline is just not necessary.
Generally IPA as solvent for extracting something from water works only if the water layer is completely saturated by salts like NaCl for example, by something what is NOT also soluble in IPA like NaOH.

See page 20 and page 30 of the attached thesis by Jademyr

 

[mithyl2]

Any concentration of NaOH will do as long you get to ph 12. More diluted like 10% and cold from the fridge is better and adding it to the reaction which has cooled down too as it easily possible to burn, say destroy some of your product by adding strong lye to a hot A-solution. Same for adding acid, diluted and cold. If your HCl was diluted and everything coldish at least then it will be fine.
Well yes, fish it is, thats the smell of A.
You want the solution you steamdistill at ph 12 but not choke-full with NaOH as otherwise when the water gets less one easily blows over some NaOH and this you do not want in your A. The filtration is done as it sems some Boron stuff likes to steamdistill over - this you also do not want.

OrgUnikumok. I'm steam distilling (or trying to) as I'm type this. A problem i'm having is the enormous fluctuation in the temperature of the steam. a change in 1 degree on the mantle can increase or reduce by 15+ degrees on the steam.

I think the fishy smell is the naoh, (it is the same as when i attempted a dmt extraction).

 

[OrgUnikum]

ok. I'm steam distilling (or trying to) as I'm type this. A problem i'm having is the enormous fluctuation in the temperature of the steam. a change in 1 degree on the mantle can increase or reduce by 15+ degrees on the steam.

I think the fishy smell is the naoh, (it is the same as when i attempted a dmt extraction).

mithyl2The steam-temperature should be 94 to 98 °C you can hardly get over 100 °C so if it boils it will make steam and the steam has 94 °C+ with A and 99-100 °C with plain water.

NaOH has no smell, NaOH vapors are extremely caustic you will feel it when it eats your face.
Amines are the ones with the rotting fish stink.

 

[ethanaaa]

Hello,
Can sodium borohydride in this experiment be replaced with cas25895-60-7 Sodium cyanoborohydride?

 

[OrgUnikum]

Hello,
Can sodium borohydride in this experiment be replaced with cas25895-60-7 Sodium cyanoborohydride?

ethanaaaCyanoborohydride is very well suited for reductive aminations as it does not reduce ketones, say its less powerful then NaBH4. It is also prone to release cyanide on contact with acids and it is quite expensive. It might be just able to do the job here if in combination with Nickel Chloride, with Cu(II) I have my doubts and think rather not. It makes little to no sense to try to use it for this reaction.