HRID1084695

反应详情

EQUATION

反应方程式

HRID 1084695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 6.08 g of 2-chloro-3-methylaniline, 9 g of di(2-bromoethyl)amine hydrobromide and 4 ml of water was added a solution of 0.8 g of potassium hydorxide and 2.5 ml of water 3 times of 1 hour interval at 100° C., then the reaction mixture was stirred at the same temperature for 9 hours. To the resultant reaction mixture was added potassium hydroxide to make the mixture alkaline, and the mixture was extracted with diethyl ether, washed with water, dried with anhydrous magnesium sulfate. The solvent was removed by evaporation and the residue thus obtained was purified by means of a silica gel column chromatography (eluent: 5%-methanol/chloroform), and obtained 3.41 g of 4-(2-chloro-3-methylphenyl)piperazine.

WORKUP

后处理

  1. customTo the resultant reaction mixture
  2. extractionthe mixture was extracted with diethyl ether
  3. washwashed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was removed by evaporation
  6. customthe residue thus obtained
  7. customwas purified by means of a silica gel column chromatography (eluent: 5%-methanol/chloroform)