反应详情

温度

93 °C

A mixture of 3,4,6-trichlorophthalic acid (25.01 g, 92.8 mmol) and glacial acetic acid (100 mL) was charged to a 250 mL 3-neck flask, equipped with a dry-ice condenser, thermometer, gas sparger and magnetic stirrer and maintained under an atmosphere of dry nitrogen. The mixture was heated and maintained at 50°-54° C. while methylamine (12 g, 0.4 mol) was introduced over a period of 1.5 hours. Following the addition of the methylamine, the reaction mixture was heated to 93° C. and maintained thereat for about 5 hours, then cooled to room temperature and filtered. The filter cake was washed with cold water and vacuum dried (0.2 mmHg) for 24 hours to yield 15.97 g of 3,4,6-trichloro-N-methylphthalimide as a white powder (m.p. 166°-167.5° C.).

1. additionwas charged to a 250 mL 3-neck flask
2. customequipped with a dry-ice condenser
3. temperaturethermometer, gas sparger and magnetic stirrer and maintained under an atmosphere of dry nitrogen
4. temperatureThe mixture was heated
5. additionwas introduced over a period of 1.5 hours
6. temperaturemaintained
7. temperaturecooled to room temperature
8. filtrationfiltered
9. washThe filter cake was washed with cold water and vacuum
10. customdried (0.2 mmHg) for 24 hours