HRID35174

反应详情

EQUATION

反应方程式

HRID 35174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.19 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide (see Example 10), 12 ml of chloroform, 2.7 ml of 50% sodium hydroxide solution and 50 mg of triethylamine is stirred at room temperature for 1 hour. The reaction mixture is then poured onto ice/water and the whole is extracted with methylene chloride. The extracts are washed with water, dried over anhydrous sodium sulphate and evaporated, and the residue is purified by flash chromatography on silica gel [eluent: n-hexane/ethyl acetate (9:1)]. There is obtained 5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile, m.p. 118°-121° C.

WORKUP

后处理

  1. additionThe reaction mixture is then poured onto ice/water
  2. extractionthe whole is extracted with methylene chloride
  3. washThe extracts are washed with water
  4. dry with materialdried over anhydrous sodium sulphate
  5. customevaporated
  6. customthe residue is purified by flash chromatography on silica gel [eluent: n-hexane/ethyl acetate (9:1)]