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.
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.
- By OrgUnikum
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
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
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- By mithyl2
OrgUnikumAfter I added the CuSO4*5H2O and then held the solution at 80c for 30 minutes, I added hydrochloric acid in the absence of acetic acid (that should be ok?) so the solution reached ph 2, and then I used simple distillation to distill off the IPA between the temps of 83C - 91C (although virtually nothign came over past about 87c), then cooled down the solution, filtered it, then added the aqueous NaOH. Now at this point I'll steam distill the amphetamine out. Do let me know if there's anything wrong with the order of things here. (I don't think I needed to filter the solution and I'll need to reflux the solution for about 3 hours instead of holding it at 80C for 30 mins.)
When I filtered the solution to separate the copper complex and I added the aqueous NaOH and the solution turned dark murky brown and smelled a little of fish with a ph of 11, and the copper was a green cake substance. I'll add more aqueous NaOH to increase to ph 12, then I'll steam distill from here. (No layers formed upon the naoh addition, so it appears i've got rid of all of the ipa from the solution.)
might toluene be a good candidate for a water insoluble nonpolar solvent?
With regards to basifying the reaction, are you saying that 20% NaOH is overkill, and that 10% will do?
When I filtered the solution to separate the copper complex and I added the aqueous NaOH and the solution turned dark murky brown and smelled a little of fish with a ph of 11, and the copper was a green cake substance. I'll add more aqueous NaOH to increase to ph 12, then I'll steam distill from here. (No layers formed upon the naoh addition, so it appears i've got rid of all of the ipa from the solution.)
might toluene be a good candidate for a water insoluble nonpolar solvent?
With regards to basifying the reaction, are you saying that 20% NaOH is overkill, and that 10% will do?
- By OrgUnikum
mithyl2Any 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.
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.
- By mithyl2
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).
I think the fishy smell is the naoh, (it is the same as when i attempted a dmt extraction).
- By OrgUnikum
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.
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.
I know the problems