HRID2051344

反应详情

EQUATION

反应方程式

HRID 2051344 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.6 g (0.043 mol) of 8-chloro-1,1-dimethyl -1,2,3,4,5,6-hexahydrobenzo[f]quinoline and 6.6 ml (0.047 mol) of triethylamine are dissolved in 100 ml of methylene chloride and 3.5 ml (0.047 mol) of acetyl bromide dissolved in 20 ml of methylene chloride are added dropwise thereto at 0°. After stirring for 1 hour, the mixture is extracted with methylene chloride/water, dried with magnesium sulfate and the solvent is distilled in a vacuum. Recrystallization from methylene chloride/ hexane gives 4-acetyl-8-chloro-1,1-dimethyl-1,2,3,4,5,6hexahydrobenzo[f]quinoline as white crystals with melting point 126-127°.

WORKUP

后处理

  1. additionare added dropwise
  2. customat 0°
  3. extractionthe mixture is extracted with methylene chloride/water
  4. dry with materialdried with magnesium sulfate
  5. distillationthe solvent is distilled in a vacuum
  6. customRecrystallization from methylene chloride/ hexane