One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)
- Thread starter GhostChemist
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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.
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.
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.
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 ?
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 ?
Hi. 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.
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.
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.
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 ...
I 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.
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.