3-CMC SOLVENT QUESTION

Researcherr

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Greetings all the forum members!

Can anyone please share the secret of solvent with 3-CMC synthesis
Which solvent to use? NMP, DSMO, Ethyl acetate, DCM?

Someone here had to do this synthesis and knows the correct solvent.

Please help!
 

G.Patton

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Hi. Same as for 4-MMC.
 

Jesse_Pinkman_

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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
 

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sierraleone

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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
Jesse_Pinkman_

Stick to this method.
Use NMP, DMF or DMSO.
 
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