Hello,
Here is the summary of a MDA via AA and NaBH4 try, all quantities according to labtop ratios:
1) AA, 50 gr MDP2P, MeOH, silicagel, no inert gaz, but stoppered flask. 8hours under slow stiring. Yellow color at the end.
2) NaBH4, added over 1h30, temp never past 10°C. New silicagel. No inert gaz, stoppered. 36h slow steering at room temp (~17°C). Final color: yellow-orange, not red.
3) Added approx. 800ml 5% NaOH. Extract the MDA/remaining MDP2P with DCM.
Error 1: no acid washes
4) Distilled off DCM, distilled freebase/MDP2P at 120°C at 3 Torr. Result: 30gr product.
5) Diluted the freebase/MDP2P in approx. 500ml IPA. Gaz up to acid pH. NO CRYSTALS
Error 2: Too much IPA
6) Distilled half of the IPA, nice crystals in the remaining. Result after drying and washing: 7gr MDA
BIG QUESTION:
It seems that I have a remaining mix of MDA/acidified-old-MDP2P/IPA in my flask. Maybe the crystals are not forming due to the presence of the MDP2P. What can I do to isolate my MDA
The smell of MDA is strongly present in this mix.