Triethylamine → HCID 22917218, compound

Participants

Reaction Steps

A solution of 4-methoxy-o-phenylenediamine (9.5 g) and triethylamine (7 g) in ethanol (100 ml) was cooled to 0°-5° and stirred in an atmosphere of nitrogen. Diethyl bromomalonate (23.7 g) in ethaol (50 ml) was added during 30 minutes. The temperature of the mixture was maintained at 0°-5° for a further 6 hours and then allowed to rise to 20° and stirred at this temperature for 16 hours. The solid was filtered off, stirred with dilute hydrochloric acid (400 ml., 0.2N), filtered off, washed with water, dried and crystallised from a mixture of ethyl acetate and methanol, m.p. 229°.

Provenance & Evidence