HRID441990

反应详情

EQUATION

反应方程式

HRID 441990 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 pulverized calcium chloride are saturated with hydrochloric acid gas over a period of 21/2 hours at 15° and subsequently stirred for an additional 3 hours. After the addition of 0.8 g. of activated charcoal, the mixture is filtered and washed with benzene. The benzene phase is evaporated under reduced pressure, whereby there is obtained 10-chloro-10,11-dihydro-3-methoxy-8-(methylthio)-dibenzo[b,f]thiepin, having a melting point of 120°-123°.

WORKUP

后处理

  1. additionAfter the addition of 0.8 g
  2. filtrationof activated charcoal, the mixture is filtered
  3. washwashed with benzene
  4. customThe benzene phase is evaporated under reduced pressure