HRID962552

反应详情

EQUATION

反应方程式

HRID 962552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

As described in Example 9, 0.471 g (1.5 mmol) of 5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine is reacted with 0.315 g (1.8 mmol) of 2-chlorobenzoyl chloride in dichloromethane. The product is chromatographed on thick layer silica gel plates with hexane-ethyl acetate (1:1) as solvent to give a solid. Recrystallization from hexane-dichloromethane gives 100 mg of crystals, m.p. 110°-115° C. Anal. Calc'd for C28H21ClN2 O2 1/2 H2O: C,72.8; H,4.8; N,6.1; Cl,7.7. Found: C,72.6; H,4.5; N,5.8; Cl,8.7.

WORKUP

后处理

  1. customThe product is chromatographed on thick layer silica gel plates with hexane-ethyl acetate (1:1) as solvent
  2. customto give a solid
  3. customRecrystallization from hexane-dichloromethane