HRID1156285

反应详情

EQUATION

反应方程式

HRID 1156285 的结构方程式

PROCEDURE

实验过程

A solution of 33 g of 11-hydroxy-6,11-dihydrodibenz[b,e]thiepin in 400 ml of absolute alcohol is saturated with hydrogen chloride gas at 5° C. for 1/2 hour. The resulting solution is dried with CaCl2, filtered and concentrated in vacuo to an oil which crystallizes upon standing in a refrigerator (10° C.) after 3 days. Recrystallization from cyclohexane provides 27 g of 11-chloro-6,11-dihydrodibenz[b,e]thiepin m.p. 79°-82° C.

WORKUP

后处理

  1. dry with materialThe resulting solution is dried with CaCl2
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo to an oil which
  4. customcrystallizes
  5. customRecrystallization from cyclohexane