HRID1441113

反应详情

EQUATION

反应方程式

HRID 1441113 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5.00 g of 4'-bromo-4-chlorobutyrophenone in 3 ml of toluene was added 11.1 ml of di-n-hexylamine and heated under reflux for 3 hours. After diluting with toluene, the reaction mixture was extracted with a 2N aqueous solution of hydrochloric acid. The extract was neutralized with a mass of sodium hydroxide and extracted with methylene chloride. Next, after drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, thereby giving 4.88 g of crude 4'-bromo-di-n-hexylaminobutyrophenone.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. extractionthe reaction mixture was extracted with a 2N aqueous solution of hydrochloric acid
  4. extractionextracted with methylene chloride
  5. dry with materialNext, after drying over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure