3-CMC Synth for a Newbie

[Jesse_Pinkman_]

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 , 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

 

[acidtobase125]

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 , 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

Jesse_Pinkman_Hi I'm very glad you are sharing your experience I have a few questions

What is the efficiency of this method ?

Is it possible to transfer it to plastic barrels to scale up to kilograms of finished product if so how to do it ?

For the help received, I will be happy to repay you when everything at my place starts greetings

 

[sierraleone]

Lol, this picture is 3cmc of india.

Sjeik>india
>Straigh out of methylamine 40% ganges water solution.

 

[salamanco]

What is 2b3c? I got everything else but I'm not sure about what that is. Sorry if this is a dumb question

 

[Precursor-supplier]

2-Bromo-3'-chloropropiophenone 34911-51-8

 

[salamanco]

2-Bromo-3'-chloropropiophenone 34911-51-8

Precursor-supplierThank you!