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
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
if we use ethyl acetate no need to heat?
need to shake for 20 minutes?
if we use ethyl acetate no need to heat?
need to shake for 20 minutes?
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