HRID2169356

反应详情

EQUATION

反应方程式

HRID 2169356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(4-chlorophenyl)-cyclopentyl]-methanol (319) (12 g, 56.95 mmol) in dichloromethane (110 mL) was added triethyl amine (16 mL, 113.90 mmol) followed by mesyl chloride (5.3 mL, 68.34 mmol) at 0° C. The reaction mixture was stirred at room temperature for 4 h, diluted with dichloromethane (50 mL) and washed with water (100 mL), saturated aqueous sodium bicarbonate solution (50 mL) and brine (50 mL). The organic part was dried, concentrated and purified by CombiFlash column (eluted at 10-20% ethyl acetate in hexane) to get methanesulfonic acid 1-(4-chlorophenyl)-cyclopentylmethyl ester (320) (14 g, 85%) as a light yellow crystalline solid.

WORKUP

后处理

  1. washwashed with water (100 mL), saturated aqueous sodium bicarbonate solution (50 mL) and brine (50 mL)
  2. customThe organic part was dried
  3. concentrationconcentrated
  4. custompurified by CombiFlash column (eluted at 10-20% ethyl acetate in hexane)