so, my experience is,
100g 2b3c
300dcm
200methylamin40% aqua
3 hours stirring
I use a sealed glas 1,8l, put foil between lid and glass so that nothing smells or gas escapes.
After reaction took place
2 times washing with dest.water
1 time extract water phase with dcm
put into rm,
add same amount fresh water into rm
put on magnetic stirrer
acidificaction drop by drop till ph6, about 50-55ml HCI,
after that take the water layer,evaporate the, let it crystallize, takes some time
opt. rotovap till 50% of the water is gone, then air drop
ethylacetat is possible, takes only 20 min, no heating necessary, rest same prosedure like with dcm
I waited min 2 days untill crystals began to form, these on the picture have not been washed with acetone but after that they are like glass. Very nice