patrick (Stranger)
02-22-02 09:35
No 272081
      MDA/NaBH4 problem-help needed !  Bookmark   

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 10C. New silicagel. No inert gaz, stoppered. 36h slow steering at room temp (~17C). 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 120C 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.
 
 
 
 
    Osmium
(Stoni's sexual toy)
02-22-02 09:41
No 272082
      Re: MDA/NaBH4 problem-help needed !  Bookmark   

Do the A/B:
Remove the bulk of your IPA by distillation. Flood the residue with water. Acidify with HCl. Not pH 6.8 or some such bullshit, make it real acidic. Wash 3 times with your favorite NP. Then basify with strong NaOH. The freebase will come out. Extract three times with your favorite NP. Then either gas it with HCl gas, OR evap the NP, take up the freebase in approx 3-4 times its weight in IPA, gas it, then add lots of acetone. Crystals.

I'm not fat just horizontally disproportionate.
 
 
 
 
    patrick
(Stranger)
02-22-02 10:51
No 272106
      Re: MDA/NaBH4 problem-help needed !  Bookmark   

Thanks for the answer.
Do I have to hurry or can I wait 3 days before to proceed?
 
 
 
 
    hest
(Hive Bee)
02-22-02 11:13
No 272111
      Re: MDA/NaBH4 problem-help needed !  Bookmark   

hurry hurry hurry !!