反应详情

To a warm (55°-60° C.) solution of 250 ml. of thionyl chloride and 50 ml. of chloroform and 6 drops of pyridine is added 3-(chloroacetylamino)benzoic acid (150 g., 0.702 mole) in 3 equal portions at 0.5 hr. intervals. After the addition is complete, the reaction mixture is warmed to a temperature of 55°-65° C. for 2 hrs., cooled and diluted with 500 ml. of petroleum ether (b.p. 30°-60° C.). The precipitate which forms is collected, washed with petroleum ether (b.p. 30°-60° C.) and dried under vacuum over potassium hydroxide at room temperature to afford 143 g. (80% yield) of 3-(chloroacetylamino)benzoyl chloride, m.p. 106°-108° C.

1. temperatureTo a warm (55°-60° C.) solution of 250 ml
2. additionAfter the addition
3. temperaturethe reaction mixture is warmed to a temperature of 55°-65° C. for 2 hrs
4. temperature, cooled
5. additiondiluted with 500 ml
6. customThe precipitate which forms is collected
7. washwashed with petroleum ether (b.p. 30°-60° C.)
8. dry with materialdried under vacuum over potassium hydroxide at room temperature
9. customto afford 143 g