Hello everyone!
This will be my first post on the forum so help me out!
I am just glad ive finally found a community that may be able to assist me, as a third year chem student I still have practically nobody who shares the same interests as me. Anyway...
I am very tired so forgive my patchy description but I will do my best (its 6am here)
I had this dream the other night...
Mercury nitrate was prepared by dissolving 200mg of mercury in approx 5ml of 70% nitric acid, and allowed to dissolve.
500ml of IPA was put in a beaker in an oil bath in order to heat to boiling.
100ml of GAA was made up to 150ml (60%w/v) and added to a 1L 2-neck RBF with condenser set up for reflux.
10g of P2NP was then dissolved in approx 60-100ml of hot IPA, then placed in an ice bath to cool in order for recrystallization to occur.
25g of pre-prepared aluminium foil cut into 3x3cm squares were scrunched into loose balls, and about 1/2 of them added to the flask, along with a stirbar.
The beaker now containing recrystallized P2NP was then taken, dirty IPA removed to a recycle container, and the freshly recrystalized P2NP dissolved in the remaining hot IPA.
3/4 of this hot IPA/P2NP mixture was then added to the reaction flask, and magnetic stirring begun.
The nitric acid/mercury nitrate was then added to the flask with a funnel, and the residue stuck to the funnel washed down into the reaction matrix with the remaining hot IPA/P2NP mixture.
The second neck was plugged and water began running to the attached condenser.
After 10 minutes the amalgamation was obvious with the liquid changing slowly becoming more opaque.
The reaction was allowed to sit for an hour and a half, when the rest of the aluminium foil was added.
This mixture was allowed to stir for 8 hours (way longer than neccisary but I had to leave it..)
The resulting grey porridge was vacuum filtered (it was a hassle!!) and the filter cake was carefully disposed of.
The remaining liquid should contain a mixture of IPA, GAA, Amphetamine, and bi-products.
THIS IS WHERE MY QUESTIONS BEGIN.
I have seen all sorts of different methods from where to go from here, so im going to discuss a few things that have and haven't worked for me.
Originally, i basified this mixture with NaOH solution until two layers formed, the bottom being aqueous, and the top being IPA and amphetamine freebase. I then separated this top layer into a clean, dry beaker, and slowly added a solution of (1:5 ratio of IPA + 98% H2SO4) until pH 7 was reached. To this suspension 100ml of chilled anhydrous acetone was added and the mixture was put in a freezer to cool.
This was then vacuum filtered to yeild 3g of dirty amphetamine sulfate.
This salt was then dissolved in a minimal amount of dH2O, filtered to remove non-soluble impurities, then washed with 20ml of Toluene. The toluene was then discarded, and the water layer added to a separate beaker. To this beaker was then added 100ml of IPA and then basified with NaOH solution. The top layer (now containing IPA and freebase) was then separated, then re-salted to a pH 7, and then 100ml of acetone was added. This yeilded 2.4g of amphetamine sulfate.
This is a less than ideal workup with a very low yield.
SO MY QUESTION IS. Instead of this method of salting, I want to evap the solvent from the freebase to get the residue in order to see the amount of amphetamine freebase I am getting. I have read:
"The obtained grey porridge in which there still was some unreacted aluminium was cooled and cautiously basified with 500 g KOH in 500mls water. Two layers formed: the lower, aqueous, with some unreacted hydroxides and the upper, consisting of IPA and the product. The mixture was extracted with 2x150 mls ether, the pooled extracts dryed and the solvent stripped off at rotovap. 25 g of crude amphetamine base was obtained as a muddy (inorganics) liquid of skin color."
First of all, how does he extract the freebase into ether when ether is miscible in IPA? Foolishly I attempted this by adding ether to the IPA/Freebase mixture, only to find the ether was miscible with the IPA and there was no was I could separate the ether from IPA. So I couldnt evaporate the ether it to leave the residue as I had planned.
What is the best way to extract the freebase from the IPA+Freebase mixture? I am thinking next time I will separate the IPA + amphetamine freebase layer from the aqueous layer, then extract the freebase into Toluene by shaking the IPA+Freebase layer with 100 ml of toluene, separate the toluene, then distill toluene which should leave this residue? In which I can dissolve the freebase residue in IPA and salt from there, hopefully obtaining a more pure product.
So basically
Once I have a freebase in IPA, how do I extract it into a solvent so that I can evaporate the solvent leaving the freebase residue?
And is this the best way of purifying the amphetamine? I figure by extracting it into a non-polar, you will remove polar impurities. I am trying to avoid distillation of the freebase because I am attempting this with 10g batches only, and distilling only a few mls of freebase would be agitating.
Please share with me your thoughts on the best way to obtain a pure product from the freebased post reaction fluid.
I feel until I work this out I wont stop having this horrible dream =.='
Thanks!
This will be my first post on the forum so help me out!
I am just glad ive finally found a community that may be able to assist me, as a third year chem student I still have practically nobody who shares the same interests as me. Anyway...I am very tired so forgive my patchy description but I will do my best (its 6am here)
I had this dream the other night...
Mercury nitrate was prepared by dissolving 200mg of mercury in approx 5ml of 70% nitric acid, and allowed to dissolve.
500ml of IPA was put in a beaker in an oil bath in order to heat to boiling.
100ml of GAA was made up to 150ml (60%w/v) and added to a 1L 2-neck RBF with condenser set up for reflux.
10g of P2NP was then dissolved in approx 60-100ml of hot IPA, then placed in an ice bath to cool in order for recrystallization to occur.
25g of pre-prepared aluminium foil cut into 3x3cm squares were scrunched into loose balls, and about 1/2 of them added to the flask, along with a stirbar.
The beaker now containing recrystallized P2NP was then taken, dirty IPA removed to a recycle container, and the freshly recrystalized P2NP dissolved in the remaining hot IPA.
3/4 of this hot IPA/P2NP mixture was then added to the reaction flask, and magnetic stirring begun.
The nitric acid/mercury nitrate was then added to the flask with a funnel, and the residue stuck to the funnel washed down into the reaction matrix with the remaining hot IPA/P2NP mixture.
The second neck was plugged and water began running to the attached condenser.
After 10 minutes the amalgamation was obvious with the liquid changing slowly becoming more opaque.
The reaction was allowed to sit for an hour and a half, when the rest of the aluminium foil was added.
This mixture was allowed to stir for 8 hours (way longer than neccisary but I had to leave it..)
The resulting grey porridge was vacuum filtered (it was a hassle!!) and the filter cake was carefully disposed of.
The remaining liquid should contain a mixture of IPA, GAA, Amphetamine, and bi-products.
THIS IS WHERE MY QUESTIONS BEGIN.
I have seen all sorts of different methods from where to go from here, so im going to discuss a few things that have and haven't worked for me.
Originally, i basified this mixture with NaOH solution until two layers formed, the bottom being aqueous, and the top being IPA and amphetamine freebase. I then separated this top layer into a clean, dry beaker, and slowly added a solution of (1:5 ratio of IPA + 98% H2SO4) until pH 7 was reached. To this suspension 100ml of chilled anhydrous acetone was added and the mixture was put in a freezer to cool.
This was then vacuum filtered to yeild 3g of dirty amphetamine sulfate.
This salt was then dissolved in a minimal amount of dH2O, filtered to remove non-soluble impurities, then washed with 20ml of Toluene. The toluene was then discarded, and the water layer added to a separate beaker. To this beaker was then added 100ml of IPA and then basified with NaOH solution. The top layer (now containing IPA and freebase) was then separated, then re-salted to a pH 7, and then 100ml of acetone was added. This yeilded 2.4g of amphetamine sulfate.
This is a less than ideal workup with a very low yield.
SO MY QUESTION IS. Instead of this method of salting, I want to evap the solvent from the freebase to get the residue in order to see the amount of amphetamine freebase I am getting. I have read:
"The obtained grey porridge in which there still was some unreacted aluminium was cooled and cautiously basified with 500 g KOH in 500mls water. Two layers formed: the lower, aqueous, with some unreacted hydroxides and the upper, consisting of IPA and the product. The mixture was extracted with 2x150 mls ether, the pooled extracts dryed and the solvent stripped off at rotovap. 25 g of crude amphetamine base was obtained as a muddy (inorganics) liquid of skin color."
First of all, how does he extract the freebase into ether when ether is miscible in IPA? Foolishly I attempted this by adding ether to the IPA/Freebase mixture, only to find the ether was miscible with the IPA and there was no was I could separate the ether from IPA. So I couldnt evaporate the ether it to leave the residue as I had planned.
What is the best way to extract the freebase from the IPA+Freebase mixture? I am thinking next time I will separate the IPA + amphetamine freebase layer from the aqueous layer, then extract the freebase into Toluene by shaking the IPA+Freebase layer with 100 ml of toluene, separate the toluene, then distill toluene which should leave this residue? In which I can dissolve the freebase residue in IPA and salt from there, hopefully obtaining a more pure product.
So basically
Once I have a freebase in IPA, how do I extract it into a solvent so that I can evaporate the solvent leaving the freebase residue?
And is this the best way of purifying the amphetamine? I figure by extracting it into a non-polar, you will remove polar impurities. I am trying to avoid distillation of the freebase because I am attempting this with 10g batches only, and distilling only a few mls of freebase would be agitating.
Please share with me your thoughts on the best way to obtain a pure product from the freebased post reaction fluid.
I feel until I work this out I wont stop having this horrible dream =.='
Thanks!
72.pdf
, its also possible to make p2p from it. Disolve your p2np in water (or MeOH) add reflux some Fe and hcl (slowly, it just fucked my lab roof, whent squirted out of reflux cooler), then steam destill your nice p2p. 