反应详情

温度

60 °C

To a solution of 3.2 kgs. isatoic anhydride in 15 kgs. dimethylacetamide is added under nitrogen with stirring sodium hydride obtained from 880 gms. of a 57% dispersion in mineral oil, while maintaining the temperature below 25°C. The resulting mixture is heated to about 60°C. and held at about 55°-60°C. for 1 hour. The reaction mixture is then cooled to 20°-30°C. and to it is added 3.0 kgs. p-fluorobenzyl chloride. The mixture is then reheated to about 60°C. and held there for about 4 hours. It is then cooled again to 20°C. and to it is added 17.4 kgs. of ice and then 24 kgs. water. The mixture is stirred for 15 minutes, the solids collected by filtration, washed with several 2 kg. portions of water and then three times with 0.7 kg. diethylether. The washed solids are dried to obtain N-(p-fluorobenzyl)isatoic anhydride, m.p. 140°-143°C.

1. customobtained from 880 gms
2. temperatureof a 57% dispersion in mineral oil, while maintaining the temperature below 25°C
3. temperatureThe reaction mixture is then cooled to 20°-30°C. and to it
4. additionis added 3.0 kgs
5. customis then reheated to about 60°C.
6. waitheld there for about 4 hours
7. temperatureIt is then cooled again to 20°C. and to it
8. additionis added 17.4 kgs
9. filtrationthe solids collected by filtration
10. washwashed with several 2 kg
11. customThe washed solids are dried