Performed the procedure twice, first time did not work (I believe from failed aluminum amalgam)
2nd procedure used the following procedure:
1. 10 gr foil, cut to 3x3 cm was amalgamated in solution of 200 mg mercuric chloride in 400 ml warm water until solution became greish and bubbles formed at surface.
2. Water was decanted and aluminum amalgam washed twice with 250 ml cold water
3. To the aluminum amalgam, the following were added quickly: 43 ml methylamine aqueous 40%, 100 ml IPA, 13.4 ml P2P, then another 100 ml IPA.
4. The aluminum pieces were poked with a rod so they stay below the surface of the liquid. Bubbles formed quickly and temperature rose. Flask was immersed in cold water bath when temp reaches over 50C
5. At the 2 hour mark, most of the aluminum was consumed, and 20 ml 25% sodium hydroxide solution was added with stirring, making sure temp does not exceed 50C, then after 3 hours, another 20 ml 25% sodium hydroxide solution was added (5 gr sodium hydroxide in 20 ml water)
6. Reaction was stirred overnight, room temp, then allowed to settle
7. The clear layer was decanted and saved, then 100 ml IPA was added to the grey sludge then stirred for another hour then decanted the IPA layer after particles settled. The aluminum sludge was then vacuum filtered and washed with 2x 50 ml methanol, then all decantations and filtrate were saved
8. Wash with 75 ml brine (25% sodium chloride solution in water) then dry with sodium sulfate with magnetic stirring for 15 mins, then filter
9. Heat the solution to 110C to remove all solvents
10. to the freebase meth, add 150 ml ethanol then add HCl in IPA solution until ph 6
11. Filter the crystals
We acquired crystals from the procedure, a bit bitter, salty crystals.
The melting point of the crystal is very high, it wouldn't roll down the foil after heating, although insufflation and oral both are highly psychoactive with good feedback.
Will be doing A/B extraction on the crystals to see if we can cut out whatever is making it have high melting point
White crystals that were filtered and dried:
After single solvent recrystallization:
anyone have thoughts on what caused the crystal to have high melting point?
2nd procedure used the following procedure:
1. 10 gr foil, cut to 3x3 cm was amalgamated in solution of 200 mg mercuric chloride in 400 ml warm water until solution became greish and bubbles formed at surface.
2. Water was decanted and aluminum amalgam washed twice with 250 ml cold water
3. To the aluminum amalgam, the following were added quickly: 43 ml methylamine aqueous 40%, 100 ml IPA, 13.4 ml P2P, then another 100 ml IPA.
4. The aluminum pieces were poked with a rod so they stay below the surface of the liquid. Bubbles formed quickly and temperature rose. Flask was immersed in cold water bath when temp reaches over 50C
5. At the 2 hour mark, most of the aluminum was consumed, and 20 ml 25% sodium hydroxide solution was added with stirring, making sure temp does not exceed 50C, then after 3 hours, another 20 ml 25% sodium hydroxide solution was added (5 gr sodium hydroxide in 20 ml water)
6. Reaction was stirred overnight, room temp, then allowed to settle
7. The clear layer was decanted and saved, then 100 ml IPA was added to the grey sludge then stirred for another hour then decanted the IPA layer after particles settled. The aluminum sludge was then vacuum filtered and washed with 2x 50 ml methanol, then all decantations and filtrate were saved
8. Wash with 75 ml brine (25% sodium chloride solution in water) then dry with sodium sulfate with magnetic stirring for 15 mins, then filter
9. Heat the solution to 110C to remove all solvents
10. to the freebase meth, add 150 ml ethanol then add HCl in IPA solution until ph 6
11. Filter the crystals
We acquired crystals from the procedure, a bit bitter, salty crystals.
The melting point of the crystal is very high, it wouldn't roll down the foil after heating, although insufflation and oral both are highly psychoactive with good feedback.
Will be doing A/B extraction on the crystals to see if we can cut out whatever is making it have high melting point
White crystals that were filtered and dried:
After single solvent recrystallization:
anyone have thoughts on what caused the crystal to have high melting point?
- By OrgUnikum
rothschild33Guys, you have such nice expensive equipment why the bloody fuck don't you get yourself decent Al-granules but use fucking foil? My Al/Hgs never worked well until I started using granules but then like a charm! The stuff is cheap and unwatched. Do not use foil. If you really want try it later with foil but if you have a good stirrer like you have - foil makes zero sense but fucking up everything. If you have no good stirrer well, thats an excuse but no, better not. Its not just me telling this, look over the old boards in the end everybody tells you to use "Good Al" and this means NOT FOIL.
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OrgUnikumUsing thicker foil on 10L plus batches, especially on a pressure vessle works perfect.
1 bar 10 temp higher, suggest nitro instead of methylamine but be sure to wash it out with saturated NaCL and baking soda, if lye is added to meta/nitro solvent saves you distilation if using hexane.
1 bar 10 temp higher, suggest nitro instead of methylamine but be sure to wash it out with saturated NaCL and baking soda, if lye is added to meta/nitro solvent saves you distilation if using hexane.
