HRID1973092

反应详情

EQUATION

反应方程式

HRID 1973092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.7 G. of 10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-ol, 250 ml. of benzene and 6 g. of finely powdered calcium chloride are saturated with hydrogen chloride gas at 15° C. within 2.5 hours and then stirred for an additional 3 hours. After the addition of 0.8 g. of active carbon, the precipitate is removed by filtration and washed with benzene. The benzene phase is evaporated under reduced pressure, and there is obtained 10-chloro-10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin having a melting point of 120°-123° C.

WORKUP

后处理

  1. additionAfter the addition of 0.8 g
  2. customof active carbon, the precipitate is removed by filtration
  3. washwashed with benzene
  4. customThe benzene phase is evaporated under reduced pressure