HRID1794001

反应详情

EQUATION

反应方程式

HRID 1794001 的结构方程式

PROCEDURE

实验过程

4-Cyclohex-1-en-1-yl-3-methyl-benzoic acid of Step C (0.360 g, 1.66 mmol) and 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine (0.337 g, 1.83 mmol) were reacted in the manner of Example 15, Step D. Purification by flash column chromatography on silica gel, eluting with 20% ethyl acetate in hexane, followed by recrystallization from 1:1 ethyl acetate/petroleum ether afforded the title compound (0.510 g) as white crystals, m.p. 182–183° C.

WORKUP

后处理

  1. customPurification by flash column chromatography on silica gel
  2. washeluting with 20% ethyl acetate in hexane
  3. customfollowed by recrystallization from 1:1 ethyl acetate/petroleum ether