I think you have to use the 4mmc synthesis but use 2-bromo-3-chloropropiophenone instead of 2-bromo-4-methylpropiophenone, plz tell me if I am wrong
send me 9999999999999€ BTC I will tell you how to make a synthesis of 3cmc 
- By mocnykutas
3cmc if u want made synthesis is no the same like u Want made 4mmc.
Somebody WHO say is the same they say bulshit
Somebody WHO say is the same they say bulshit
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
When use EA, top layer is organic, bottom water
When use dcm its opposite
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
But i have to say yeald is not very good, maybe 20-30%
I dont know why.
What are your yealds from 100g 2b3c?
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
When use EA, top layer is organic, bottom water
When use dcm its opposite
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
But i have to say yeald is not very good, maybe 20-30%
I dont know why.
What are your yealds from 100g 2b3c?
Attachments
- By quarku
Hi, could You be more precise about some details?
How much time reaction need to finish, what it means to wash it?
My experience is just making some dmt from mhrb, can I handle that?
How much time reaction need to finish, what it means to wash it?
My experience is just making some dmt from mhrb, can I handle that?
Reaction time is mentioned in my text.
Depends on solvent.
But the whole process(with acidification ,etc) can be done in 4-5 hours (DCM) or 2 hours (ethylacetate).
Icecold acetone is used to remove some impurities, that is called washing. Works with buchner filter+Vakuum pump and also with coffee filters and funnel only with gravitation
Depends on solvent.
But the whole process(with acidification ,etc) can be done in 4-5 hours (DCM) or 2 hours (ethylacetate).
Icecold acetone is used to remove some impurities, that is called washing. Works with buchner filter+Vakuum pump and also with coffee filters and funnel only with gravitation
