Carbamic acid, ethyl ester → HCID 13765534, compound

Participants

Reaction Steps

35 g of crotonaldehyde are added dropwise at 60°-83° C. to a mixture of 133.5 g of ethyl carbamate, 15 g of acid ion exchanger resin (Duolite C 265), 0.2 g of hydroquinone monomethyl ether and 200 ml of trichloroethylene in the course of 20 minutes, and the mixture is thereafter left at 80° C. for 30 minutes. The catalyst is filtered off, the solvent is distilled off and the residue is crystallized from ethyl acetate/petroleum ether. This gives 83 g (52% yield, based on starting crotonaldehyde) of 3-methyl-1,1,3-tri(ethoxycarbonylamino)propane having a melting point of 103°-105° C.

Provenance & Evidence