HRID1614696

反应详情

EQUATION

反应方程式

HRID 1614696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Para-maleimidobenzoyl chloride was prepared in accordance with the procedure described by Adams et al. in J. Am. Chem. Soc , 42, 599 (1920). The N-(para-carboxyphenyl) maleimide (15 g) was suspended in about 80 ml of benzene with stirring. To this mixture was added 15 ml (a 2.5:1 molar excess) of oxalyl chloride, whereupon some gas was evolved. The mixture was then heated slowly to reflux and maintained at reflux for two hours. Excess oxalyl chloride was removed by distillation. The reaction mixture was then cooled and the yellow product recovered by suction filtration. The resultant product was washed with hexane and dried under vacuum at room temperature.

WORKUP

后处理

  1. additionTo this mixture was added 15 ml (a 2.5
  2. temperatureThe mixture was then heated slowly
  3. temperatureto reflux
  4. temperaturemaintained
  5. temperatureat reflux for two hours
  6. customExcess oxalyl chloride was removed by distillation
  7. temperatureThe reaction mixture was then cooled
  8. filtrationthe yellow product recovered by suction filtration
  9. washThe resultant product was washed with hexane
  10. customdried under vacuum at room temperature