4-CMC synthesis

[Crystal__Chemist]

Hi
Please someone can help with synthesis 4-cmc. Im gonna use per one mole of bromoketone 4 moles of methylamine (40% solution in water). As a solvent im gona use dcm or toluene. What is the best time and what solvent is better and what temperature should be perfect. I don't whant use benzene becouse it is verry toxic.

 

[G.Patton]

Hi, procedure is the same as for 4-MMC.

 

[Crystal__Chemist]

So if I cook it for 2 h in 40°C i will get my product in good numbers ?

 

[mocnykutas]

U Dont heat it and dcm toulen benzen ethyl acetate no work

 

[Jesse_Pinkman_]

Ethylacetate works

 

[Bazooka90]

what temperature need for ethyl acetate?

 

[Crystal__Chemist]

Can I use dmso and toluene or dcm for this reaction ?

 

[mygodson]

That patton said is correct.

 

[Crystal__Chemist]

But what solvent is better while synthesis run with dmso : dcm or tolene?

 

[UWe9o12jkied91d]

One non polar and one bipolar aprotic. for ex:

Toluene + NMP
DCM + DMSO

The point is to homogenize the mass until monophasic, this makes it go much faster.
You can alternatively react in just DCM overnight (8h)

OOPS SORRY FOR NECRO

 

[HerrHaber]

Both NMP and DMSO are water miscible high boiling (above 200*C) solvents. DCM boils notoriously low @-40*C and toluene boils @110*C. The key is the stirring.

 

[hotelier]

why even bother cooking that shite?