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]

if using HCl aqueous solution, do not dilute it with acetone. do this: after methylamination and washing the organic layer with water, add an equal volume of ethyl acetate to the organic layer (I added 16 liters of ethyl acetate). and then add undiluted HCl (40% solution in water). add hydrochloric acid and mix well until the pH is in the range of 3-6. then put the whole mass in the freezer at -20C for 15-20 hours, so that everything freezes well. at -20C, water loses its ability to dissolve 4-mmc in itself. then filter the product. output will be good.

ChemDamnCan I add acetone instead of ethyl acetate?

I left the container in the cellar completely at rest at a temperature of + 4C.

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

I must say that the method, where the reaction is carried out for 2 hours at a temperature of 40C, gives the same yield of 4-mmc. but when filtered 4-mmc it turns out brown, beige. then you have to wash it many times with acetone to wash off dirt and make it white.

Perfectly explained, praise to you for that

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.

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]

Czy mogę dodać aceton zamiast octanu etylu?


Oznacza to, że nie ma potrzeby trzymać się tych -6/-8 stopni


Doskonale wyjaśnione, chwalę za to



Czyli można bez obaw szczelnie zamknąć kolbę i tylko okresowo spuszczać nadciśnienie przez płuczkę pozbywając się zapachu? Nie wpłynie to na reakcję, wydajność lub czystość reakcji?

Prima4mmcdo 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]

Green color freebase why is ??

Didithe 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

 

[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?

 

[caesare.robot]

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