Acetic Anhydride → HCID 12912434, compound

Participants

Reaction Steps

To 14.5 ml of 90% formic acid was added 30 ml of acetic anhydride. The mixture was warmed, and then heated to 50°-60° C. for two hours. To the mixture cooled to room temperature was added portionwise with stirring 15.0 g of 2-amino-4-ethoxycarbonyl-3,5-dimethylbenzoic acid. The mixture was further stirred at room temperature for 3 hours and poured into ice water. The resulting precipitate was filtered and recrystallized from ethyl acetate/n-hexane to yield 11.8 g (70.5% of theory) of 2-formylamino-4-ethoxycarbonyl-3,5-dimethylbenzoic acid melting at 144.5°-146° C.

Provenance & Evidence