Ethyl chloroformate → Ethyl-4-chloro-5-formyl-2,3,6,7-tetrahydro-1H-1-azepine carboxylate

Participants

Reaction Steps

A solution of 3.6 gm (0.033 mol) of ethyl chloroformate in 15 ml of dry methylene chloride was added dropwise at room temperature, while stirring, within 30 minutes to a solution of 7.5 gm (0.03 mol) of 1-benzyl-4-chloro-5-formyl-2,3,6,7-tetrahydro-1H-azepine in 50 ml of dry methylene chloride, whereupon the temperature of the reaction mixture increased from 22° C. to 27° C. After the addition was complete, the mixture was stirred at room temperature for another 3 hours. Then, the methylene chloride was distilled off in a rotary evaporator, and the residue was distilled in a high vacuum.

Provenance & Evidence