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

[Mystery_chemistry]

gentlemen, how do we know what volume of 25% NaOh solution should be added? I mean where did this 8 l come from, how to calculate it?

 

[ACAB]

how to calculate it?

Mystery_chemistryFor sure there is a way to calculate it, but more important here will be the pH value, when the solution is alkaline enough to release the freebase.

 

[Mystery_chemistry]

For sure there is a way to calculate it, but more important here will be the pH value, when the solution is alkaline enough to release the freebase.

PennywiseOk, did I count well for 250g p2np that I would need 550g NaOh in 1650ml dh20? I found a dependence that the NaOh solution was added in the proportion of 44% to the amount of IPA + dh20

 

[Mystery_chemistry]

aaa and the question is what pH should be after the end of the reaction? mi shows 10-11. after adding alkali the base pops up and it is 12-13.

 

[Mystery_chemistry]

I wonder if it will not be better if in the end you will not add 50% acetic acid to get down from the pH lower and then add a little alkali to these 12… what do you think?

 

[Bartholomeus]

I wonder if it will not be better if in the end you will not add 50% acetic acid to get down from the pH lower and then add a little alkali to these 12… what do you think?

Mystery_chemistry
No need to add acetic acid, just add NaOH like stated in synthesis

 

[Mystery_chemistry]

7. The aqueous phase was thereafter extracted with 8 liters of IPA.

William Dampiergentlemen, I still did not get a reply to point 7. for me, after removing the top layer and adding to the bottom (water) IPA NOTHING HAPPENS. two layers are not formed again

 

[ACAB]

gentlemen, I still did not get a reply to point 7. for me, after removing the top layer and adding to the bottom (water) IPA NOTHING HAPPENS. two layers are not formed again

Mystery_chemistryWater and IPA also mix wonderfully, but I read from points 6 and 7 that IPA is added first and then the layer is separated. For me, the question is rather why one does not use water-insoluble petroleum ether instead of the IPA, which would keep the amount of water to be removed smaller. Drying does not take place at all here, for whatever reason ever.

 

[Mystery_chemistry]

Water and IPA also mix wonderfully, but I read from points 6 and 7 that IPA is added first and then the layer is separated. For me, the question is rather why one does not use water-insoluble petroleum ether instead of the IPA, which would keep the amount of water to be removed smaller. Drying does not take place at all here, for whatever reason ever.

Pennywisein your opinion, after adding the base and the oil flows out, IPA is added and mixed and then the top layer is pulled off?

 

[ACAB]

in your opinion, after adding the base and the oil flows out, IPA is added and mixed and then the top layer is pulled off?

Mystery_chemistryYes, that is how I understood it. Although the use of IPA does not seem optimal to me.

 

[Mystery_chemistry]

Yes, that is how I understood it. Although the use of IPA does not seem optimal to me.

Pennywiseone of the experts could explain this inaccuracy heh

 

[chemden]

hi i found some old notes regarding this p2np reduction. photo attached View attachment 5308

Mystery_chemistryCan you share this article/book?

 

[Mystery_chemistry]

why the synthesized amphetamine has no power?

everything done as it was written in the recipe. the smell is there, the taste is bitter, and the potency is very weak… what could it be?

 

[G.Patton]

why the synthesized amphetamine has no power?

everything done as it was written in the recipe. the smell is there, the taste is bitter, and the potency is very weak… what could it be?

Mystery_chemistryHave you done a/b extraction of your product? Probably, you have a lot of side products.

 

[Mystery_chemistry]

Have you done a/b extraction of your product? Probably, you have a lot of side products

G.Pattonso I did. or could it be caused by too high pH of the amine .. I think it is too alkaline. you can hardly see the difference on the strips, but it seems to me that the pH is 13-14
the next time after the reaction is complete, I will want to lower the pH with acetic or hydrochloric acid and slowly raise the pH to 12 with base.

 

[Mystery_chemistry]

to what pH is best to go down with a / b extraction to clean the amine?

 

[TerminusEst]

i want to setup everything i need to do this reaction, i am not certain about my vacuum source bc its my first time working with vacuum evaporation, i am looking at a fairly cheap Vacuum pump that is aperently pulling 5 Pa ultimate vacuum.
That is a pretty deep vacuum as far as i understand it, i am getting a 2L Cold trap and am planing to use that with water/salt ice bath to prevent IPA entering my pump but as far as i can see the deeper the vacuum is the colder my cold trap needs to be to prevent solvent entering the pump. Is it practical to just manually turn the vacuum pump of and on when the pressure gets quit low ? Looking at vacuum operations and cold traps specifically i found that quit regularly people use more than one cold trap, is this only to collect residual vapors or is there a secondary use that i dont understand ?

 

[G.Patton]

Is it practical to just manually turn the vacuum pump of and on when the pressure gets quit low ?

TerminusEstHi. You can adjust vacuum pressure by the simple split vacuum valve. And you are right concerns the dependence of cooling liquid temperature and vacuum pressure.

so I did. or could it be caused by too high pH of the amine .. I think it is too alkaline. you can hardly see the difference on the strips, but it seems to me that the pH is 13-14
the next time after the reaction is complete, I will want to lower the pH with acetic or hydrochloric acid and slowly raise the pH to 12 with base.

You don't need to adjust pH of amph oil. I told about Amphetamine purification by acid-base extraction. Probably your 13-14 pH value is method measurement error (by pH stripes), I mean that it's okay.
p.s. You don't need to use bold for answer getting.

 

[Mystery_chemistry]

thanks a lot for the reply I have one more question . what influences the formation of all these pollutants? does the temp also matter? I wonder if the reaction should not be carried out at a temperature of 55-60 degrees ... it seems to me that 80 degrees for 30 minutes causes that so much pollution is formed ...

 

[UWe9o12jkied91d]

i want to setup everything i need to do this reaction, i am not certain about my vacuum source bc its my first time working with vacuum evaporation, i am looking at a fairly cheap Vacuum pump that is aperently pulling 5 Pa ultimate vacuum.
That is a pretty deep vacuum as far as i understand it, i am getting a 2L Cold trap and am planing to use that with water/salt ice bath to prevent IPA entering my pump but as far as i can see the deeper the vacuum is the colder my cold trap needs to be to prevent solvent entering the pump. Is it practical to just manually turn the vacuum pump of and on when the pressure gets quit low ? Looking at vacuum operations and cold traps specifically i found that quit regularly people use more than one cold trap, is this only to collect residual vapors or is there a secondary use that i dont understand ?

TerminusEstI can't comment on pumps, unless it's about breaking them.I suggest you maybe look into water jet pumps? You can use the water from the tap, wasting a lot of water OR hook it up to a recirc. bath with treated water and simple water pump (you can find powerful ones for cheap).It's pretty elegant, I think mister G has a thread, aswell as Chemplayer on bitchute.
BUT If you want to do this reaction small scale simply tossing your finished, basified, cooled RM into a big sep, along with some petether, toluene, xylene, hexane few shakes, few vents badabing badaboom, repeat 3 times, pool extractions over drying agent (MgSO4, NaSO4, BaSO4 [yes, it works] , NOT CaCl2 or anything with calcium, it will gel).One thing to watch out is you want to use about as much solvent as in the procedure (scaled ofc) if organic layer is too dillute it's not gonna precipitate as readily.