HRID1649988

反应详情

EQUATION

反应方程式

HRID 1649988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 20.0 g (74 mmoles) of N-(2-bromo-butyryl)--2,6-dimethyl-aniline, 27.8 g (0.15 moles) of potassium phthalimide and 150 ml of dry dimethyl formamide is stirred at 60° C. for 2 hours. The mixture is cooled, poured onto 750 ml of ice water, the separated crystalline substance is filtered off, washed with water and dried. The resulting crude product, weighing 35.7 g, is dissolved in 200 ml of chloroform, the solution is washed thrice with 50 ml of 1 n aqueous sodium hydroxide solution and thrice with 50 ml of water, each, dried over anhydrous magnesium sulfate, and the solvent is evaporated under reduced pressure. 17.7 g (71.1%) of N-(2-phthalimido-butyryl)-2,6-dimethyl-aniline are obtained; m.p.: 195°-196° C.

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. filtrationthe separated crystalline substance is filtered off
  3. washwashed with water
  4. customdried
  5. dissolutionis dissolved in 200 ml of chloroform
  6. washthe solution is washed thrice with 50 ml of 1 n aqueous sodium hydroxide solution and thrice with 50 ml of water
  7. dry with materialeach, dried over anhydrous magnesium sulfate
  8. customthe solvent is evaporated under reduced pressure