Yield was around 70% without DCM extraction, after distillation.
View attachment 13461
- By OrgUnikum
SwesweCongratulations!
There seems to be quite some base in the water layer though, if you do not want to extract it you can add about the same amount of brine (saturated salt - NaCl - solution, easily prepared beforehand, this will press base out of the water layer and also suck some water from the base. Ideally the whole water layer would be saturated with salt but I suppose you are in a hurry so adding brine will do. You see the result after 5 to ten minutes, the water layer becoming clearer, but give it half an hour to do its job completely.
There seems to be quite some base in the water layer though, if you do not want to extract it you can add about the same amount of brine (saturated salt - NaCl - solution, easily prepared beforehand, this will press base out of the water layer and also suck some water from the base. Ideally the whole water layer would be saturated with salt but I suppose you are in a hurry so adding brine will do. You see the result after 5 to ten minutes, the water layer becoming clearer, but give it half an hour to do its job completely.
- By blackburn
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- By OrgUnikum
SwesweThats also steamdistillation, what you want to say is that you did not use an external steam-source, generator but boiled it from the reaction vessel.
Boiling point of Amphetamine Base would be around 200 °C
It is recommended to refill water in this case so there is always plenty of water around. Amphetamine base will then come with water at 94 to 98 °C measured at the stillhead/Claisen/entry of condenser.
Steamdistillation is contrary to common belief more sped up by having a wide undisturbed path for the steam then by heating like mad.
Boiling point of Amphetamine Base would be around 200 °C
It is recommended to refill water in this case so there is always plenty of water around. Amphetamine base will then come with water at 94 to 98 °C measured at the stillhead/Claisen/entry of condenser.
Steamdistillation is contrary to common belief more sped up by having a wide undisturbed path for the steam then by heating like mad.
- By btcboss2022
OrgUnikumIn case of A-oil you need an external steam source in addition to the water in the mixture to obtain the max yield, that's checked many times and always you can test it yourself. Only adding water and distill it won't obtain the max yield.
- By OrgUnikum
btcboss2022External overheated steam for sure considerably speeds the process up and I do not doubt that there will be more oil in the collection flask in the end. But I am afraid it is not more Amphetamine base but other stuff formed in the reaction. Amphetamine and Methamphetamine both distill with willingly with steam even from a just simmering flask and thats not just my imagination but it is well-documented in the literature.
This is more a point when somebody uses your base-hydrolysis method as when your acid-hydrolysis is used as in the acid hydrolysis you have a washing with DCM step before basification included which removes all non-basic unwanted stuff like leftover P2P, no such step is in the procedure with base.
Look, I want to express my gratitude for you posting this large scale method here, I seriously appreciate it very much and I want to assure you that what I write is intended to be constructive and no attempt to criticize you personally or to ridicule your abilities and achievements.
I do not know if you treat the oil from this reaction in any further ways, workup wise, for higher quality and to remove impurities or if you process it directly to "Paste" and however you do it, I am not here to judge, if your customers are happy they are happy.
For personal consumption I rather steamdistill very gently and then add some more steps but I am very old and got very sensitive to impurities in general.....
This is more a point when somebody uses your base-hydrolysis method as when your acid-hydrolysis is used as in the acid hydrolysis you have a washing with DCM step before basification included which removes all non-basic unwanted stuff like leftover P2P, no such step is in the procedure with base.
Look, I want to express my gratitude for you posting this large scale method here, I seriously appreciate it very much and I want to assure you that what I write is intended to be constructive and no attempt to criticize you personally or to ridicule your abilities and achievements.
I do not know if you treat the oil from this reaction in any further ways, workup wise, for higher quality and to remove impurities or if you process it directly to "Paste" and however you do it, I am not here to judge, if your customers are happy they are happy.
For personal consumption I rather steamdistill very gently and then add some more steps but I am very old and got very sensitive to impurities in general.....
- By btcboss2022
OrgUnikumDon't be afraid about this point I can assure you that there is more amphetamine base it's measured after solvent extraction.
In chemistry sometimes (not many) the literature differs a little from the synth reality and this is possibly one of those cases anyway I insist that you can check it yourself without problem and then comment it here.
About the solvent washing is an optional procedure since it will be steam distilled anyway and after distillation no impurities but even if you are afraid of impurities you always can make an acid-base washing when you extract the final freebase with solvent after distillation ;-)
In chemistry sometimes (not many) the literature differs a little from the synth reality and this is possibly one of those cases anyway I insist that you can check it yourself without problem and then comment it here.
About the solvent washing is an optional procedure since it will be steam distilled anyway and after distillation no impurities but even if you are afraid of impurities you always can make an acid-base washing when you extract the final freebase with solvent after distillation ;-)
