Methyl chloroformate → HCID 10466372, compound

Participants

Reaction Steps

Triethylamine (25.4 mL, 0.182 mol) was added dropwise over a 20 minute period to a cold (0°-5° C.), stirred suspension of 2-carbamoyl-4,5-dichlorobenzoic acid (21.3 g, 91.0 mmol) in dichloromethane (110 mL). Methyl chloroformate (15.5 mL, 0.2 mol) was then added dropwise over a 30 minute period. The reaction mixture was then warmed to room temperature and stirred overnight. The solvents were removed and water (200 mL) was added. The water phase was filtered and the precipitate was washed with water and dried in vacuo to provide the product (20.5 g, 97%) as a tan solid, m.p. 120°-123° C.

Provenance & Evidence