Post 189985 (missing)
(Antibody2: "Re: MDA via oxime", Methods Discourse)https://www.thevespiary.org/rhodium/Rhodium/chemistry/znhg.alhg.reductions.txt (https://www.thevespiary.org/rhodium/Rhodium/chemistry/znhg.alhg.reductions.txt)
--------------------------------------------------------------------------------
Piglet
NH2OH.HCl is readily available from photography supply. And a better reduction
using the Zn/Ni couple has been posted by labrat. Claims to reduce imines to
amines (ketone in 80% methanol saturated with NH3 at about 60-70%, yields higher
from oxime, the side-product being hydroxylamine (boo hoo!), the freebase of
which is a solid. It's active as MDA. If you really want MDA, put it right back
into the next batch being reduced!
Search for Labrats post (it IS there, I just havn't got the time) and then here
are some details. (I use the sulphate).
NiSO4 + 6NH3 --> Ni(NH3)6SO4.
Zn + H2O --> ZnO + H2.
ZnO + 4NH3 --> Zn(NH3)4(OH)2.
Pour off the NH3 solution, add your oxime in 80% v/v Methanol solution, add
3 moles of NaOH and slowly add the Zn in portions (if it overheats, cool under
running water) until it's all added, heat for 90 minutes, cool, filter (wash
filtrate into mother liquor). Neutralize, extract, remove solvent (yielding the
hydroxylamine as solid) or simply make salt as you see fit (IE a mix of MDA/MDOH).
2NaOH + Zn -->Na2[ZnO2] + 2H
--------------------------------------------------------------------------------
and Antibody2 says so :)