4mmc - amination in DCM. Some questions

[Netflix]

I see that you are doing with an open vessel during amination and then there is a very big stench throughout the process such a method leads to the police quickly rushing in and shutting down labo. the most sensible method is to keep the reactor flask closed and then the freebase does not heat up so quickly, only a maximum of 36 degrees for some time.

 

[Prima4mmc]

Can I add acetone instead of ethyl acetate?

That is, there is no need to cling to those -6/-8 degrees

Perfectly explained, praise to you for that


So it is possible to close the flask tightly without worry and only periodically bleed the excess pressure through the scrubber getting rid of the smell? This will not affect the reaction, yield or purity of the reaction?

 

[Netflix]

do as it is in the benzene video flask, stirrer and reflux condenser. the freebase will not heat up more than 36 ° C

 

[Bartholomeus]

Nice to finally see discussion of cleaner way of making mmc in progress
keep it up guys!

 

[Bennychairman]

just put a balloon on the condenser , it will keep the pressure the same in the RV

 

[Didi]

Green color freebase why is ??

 

[ChemDamn]

I can assume that you left the free base after methylamination for 15-20 hours. you can't do that. immediately after methylamination, acidification must be carried out. The 4-mmc free base is rather brittle and has a short half-life. green color - the result of decomposition and isomerization

 

[ChemDamn]

the color should be golden yellow, like a lemon, light

 

[Chemix-Express]

Green color = too much bk4 did not react, blue color = too much methylamine did not react or was not sufficiently washed out of freebase

 

[TheVacuumGuy]

Aren't those linked? I mean too much unreacted bk4 would also mean too much unreacted amine and vice versa.

 

[Bartholomeus]

After reaction, should freebase be washed 2 times with normal water, then 1 time with10% sodium bicarbonate or 1 time 10% sodium hydroxide solution?
What will make the freebase more clean? How do you people do it so that most of un-reacted bk4,methylamine, impurities are cleaned out?
After all the washes pinch of table salt is added to push the last water so it separates completely right?

 

[TheVacuumGuy]

Just do even amount of 10% sodium bicarbonate water solution (baking powder).

Then wash with even amounts of water. Shake, repeat. Until the freebase is clear not cloudy and/or water layer is clear so you'd drink it. That clean .

 

[caesare.robot]

swim strated with 4mpph. bromination via h2o2. amination with m40 in dcm. after vacuum distillation 80% freebase from starting material.