反应详情

A solution of 4-iodo-3-nitrobenzoic acid methyl ester (2.0 g, 6.5 mmol) in methanol (80 ml) is cooled to −15° C. To the solution, ammonia gas (about 1.02 g, 0.06 mol) is passed till saturation. The solution is kept at room temperature (25±2° C.) for 3 days. The solvent is then evaporated under reduced pressure to obtain 4-iodo-3-nitrobenzamide as an yellow solid (95% yield, 98% HPLC). The solid (1 g) is added to methanol (10 ml) and heated to 55° C. to get a clear solution. While the solution is hot, water (35 ml) is added and the precipitate so formed is filtered to obtain pure 4-iodo-3-nitrobenzamide.

1. customis kept at room temperature
2. custom(25±2° C.)
3. customfor 3 days
4. customThe solvent is then evaporated under reduced pressure