1,2-Dimethoxyethane → Benzoyl chloride, 3,4,5-trimethoxy-

Participants

Reaction Steps

Combine 3,4,5-trimethoxy-benzoic acid (3.5 kg, 16.5 mol) and 1,2-dimethoxyethane (14.2 kg) and dimethylformamide (4 g). Cool in an ice bath. Add oxalyl chloride (2.99 kg, 23.5 mmol) over about 50 minutes not allowing the temperature of the reaction to raise above about 19° C. After 20 hours, concentrate in vacuo at 25° C. to remove about 3.7 kg of distillate to give a solution of 3,4,5-trimethoxy-benzoyl chloride.

Provenance & Evidence