i just try this process with 1bmk :0.7 water : 0.7 h2so4 reflux 4 hours
the results was very low yield (30-40%) only .... and product was very dirty.
the best results is just dissolve the bmk in 75% h3po4 and reflux with strong heating 3 hours.
the bmk obtain in this method is very clean also...
OFC you can use mercuric nitrate...
i just bought elemental mercury and dissolve it in nitric acid (6ml/1g), then i make the amalgam by water.
25g aluminum + then i drop inside 2ml of my mercuric nitrate solution, and then i shake it occasionally for 5-10 minute or until it start bubbling nicely...
yes ... i purify dimethylamylamine first run no MgSO4 i get nice crop of white snow flakes suddenly after gas (dry by fractional distillation).
second run i used MgSO4 once i added the wet freebase to the toluene+MgSO4 solution it was cloudy, after i filter it off and gas it get nothing.
(Only...
i see that for example they use KOH to dry aniline (which is primary amine btw) for a reason i guess... (look at nile red tutorial on youtube)
i find in 2-3 sources that MgSO4 is acidic and is not recommended for amine.
btw i just successfully dry the toluene with NaOH, i use it as desiccant...
yes is used almost 20g of this stuff for 400ml toluene solvent....
i see that many of the tutorial use this much.... (20-50g per +-0.5L solvent)
why peoples use the MgSO4 if it attract amine?
NaOH Should be more suitable for dry amines ..... no ?
or i miss here something ?
Hello while purifying 1n and 2n amines i get 0% yield while bubbling hcl in toluene+amine product (50g amine in 300ml toluene) -(i used 20-30 MgSO4 to pre-dry organic phase)
i google little bit and i found that MgSO4 is incompatible with acid sensitive compounds
please check out ...