Search results

ethyl acetate

better use toluene. ethyl acetate gives a dirtier product due to gumming during the reaction of the ketone with methylamine.

depending on the method of bromination. for bromination with bromine DCM is suitable. and for bromination with HBr + perhydrol is not suitable, as the reaction is too exothermic, and DCM foams strongly and boils away

Bro, you're right. but!!! bromination can be done in dichloroethane (boiling point >75°C), but not in dichloromethane (boiling point 38.5°C).

if the solution is no longer heated, and its temperature has begun to decrease, then the reaction is complete - proceed to the next stage. the average reaction time from the start of self-heating to the temperature decrease is from 2.5 to 3.5 hours (depending on the volume of initial reagents)...

no need to close the bottle (vessel). if the temperature is not higher than 36C, then it will not stink much. the main thing is not to let the DCM boil (boiling point 38C) - then the free base will turn out to be pure, and 4-Mmc will be very pure. By the way, about crystallization: I know all...

1) no external heating is needed!!! when methylamine is added, the mixture heats up by itself (it does not heat up instantly, while stirring it takes about 5 minutes, and the temperature starts to rise). the main task is to prevent the temperature from rising above 36C. for this, methylamine...

I get the purest product in DCM, but the main thing is not to let the solution boil, keep the temperature no higher than 36C (4-mmc turns out to be impeccably clean and snow-white). Another great option is dichloroethane. also a good result is obtained when using NMP and toluene together (3:2...

Evaporate the solution until a film appears on the surface. then leave overnight in the freezer (-18/-20C). everything should crystallize

What solvent you’ve used?

Under water +1

what proportion of water/4-mmc? What is the temperature of the solution and at what temperature should the solution be left? how long does crystallization take?