HRID454161

反应详情

EQUATION

反应方程式

HRID 454161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(3-hydroxypropyl)-4-methylpiperazine (2.4 g, 15 mmol), (prepared as described for the starting material in Example 133), in dichloromethane (60 ml) was treated with triethylamine (4.6 ml, 33 mmol) and p-toluenesulphonyl chloride (3.2 g, 17 mmol) and stirred at ambient temperature for 2 hours. The solution was washed with saturated aqueous sodium hydrogen carbonate solution followed by water and filtered through phase separating paper. The filtrate was evaporated under vacuum to give 3-(4-methyl-piperazin-1-yl)propyl-4-toluene sulphonate as an oil which crystallised on standing (3.7 g, 78%).

WORKUP

后处理

  1. washThe solution was washed with saturated aqueous sodium hydrogen carbonate solution
  2. filtrationfiltered through phase
  3. customseparating paper
  4. customThe filtrate was evaporated under vacuum