HRID1414034

反应详情

EQUATION

反应方程式

HRID 1414034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Hydrogen sulphide gas was passed through a stirred solution of 3-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)ethyl]-1H-indole-5-carbonitrile (4 g) and triethylamine (3 ml) in dry dimethylformamide (100 ml) for 6 hours. and the reaction mixture was stirred for a further 7 days. Hydrogen sulphide gas was passed through the reaction mixture for 0.5 hours on each day. Water (200 ml) was added and the mixture was extracted with ethyl acetate (3×200 ml). Evaporation of the washed (H2O) and dried (MgSO4) extracts gave a yellow residue which gave a yellow powder (4.1 g) on trituration with ether. A sample was crystallised from ethanol to give the title compound as yellow microcrystals m.p. 195°-8° C. (dec.)

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (3×200 ml)
  2. customEvaporation of the
  3. washwashed (H2O)
  4. dry with materialdried (MgSO4)
  5. customextracts gave a yellow residue which