HRID582626

反应详情

EQUATION

反应方程式

HRID 582626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Thionyl chloride (2 ml) was added dropwise to a stirred, ice cooled solution of 2-[N-benzyl-N-methylamino]ethanol (4 g) obtained in preparation 8, in dry benzene (10 ml). The resulting mixture was stirred at 0° C. for 2 h and then diluted with ethyl acetate (40 ml), washed with saturated aqueous sodium bicarbonate solution (2×25 ml), water (50 ml), brine (50 ml) and dried. The ethyl acetate layer was evaporated and the residue was chromatographed on silica gel with 20% ethyl acetate in petroleum ether as eluent to give 2.6 g of the title compound.

WORKUP

后处理

  1. washwashed with saturated aqueous sodium bicarbonate solution (2×25 ml), water (50 ml), brine (50 ml)
  2. customdried
  3. customThe ethyl acetate layer was evaporated
  4. customthe residue was chromatographed on silica gel with 20% ethyl acetate in petroleum ether as eluent