HRID67640

反应详情

EQUATION

反应方程式

HRID 67640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-chloro-10,11-dihydro-5H-dibenzo[a,d]-cyclohepten-5-ylideneacetic acid (23.5 g, described in Example 1) in ethanol (100 ml, hot) is added to 5% sodium amalgam (100 g). The mixture is stirred at 60°-70° C. for 3 hr and decanted. The solution is evaporated of half its original volume, acidified with conc. hydrochloric acid and extracted with chloroform. The organic extract is dried and evaporated. The residue is crystallized from diethyl ether-hexane to give the title compound as crystals, mp 142°-146° C.

WORKUP

后处理

  1. customdecanted
  2. customThe solution is evaporated of half its original volume
  3. extractionextracted with chloroform
  4. extractionThe organic extract
  5. customis dried
  6. customevaporated
  7. customThe residue is crystallized from diethyl ether-hexane