反应详情

温度

0 °C

A solution of 3-methoxycarbonyl-5-iodobenzoic acid (3 g, 10 mmol) in thionyl chloride (2 mL) was heated for 2 hours at 60° C. The reaction mixture was cooled and concentrated in vacuo. The intermediate acid chloride was then diluted with tetrahydrofuran (10 mL) and cooled to 0° C. The mixture was then treated with a solution of 2M ammonia (20 mL, 40 mmol, methanol) and the reaction stirred for 1 hour at 0° C. The mixture was then filtered and the solvent removed in vacuo. Recrystallization from methanol afforded 2.5 g (82%) of 3-methoxycarbonyl-5-iodobenzamide, as a white solid.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated in vacuo
3. additionThe intermediate acid chloride was then diluted with tetrahydrofuran (10 mL)
4. filtrationThe mixture was then filtered
5. customthe solvent removed in vacuo
6. customRecrystallization from methanol