HRID1414035

反应详情

EQUATION

反应方程式

HRID 1414035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium hydride (0.16 g) was added to a solution of 3-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)ethyl]-1H-indole-5-carbonitrile (2.0 g) in dry dimethylformamide (40 ml) under nitrogen. After 0.5 hour. benzyl chloride was added and after a further 2 hours the mixture was diluted with water (150 ml) and extracted with ethyl acetate (3×40 ml). Evaporation of the washed (H2O) and dried (MgSO4) extract gave a red oil which was triturated with ether and then crystallised from ethanol to give the title compound as yellow microcrystals (1.2 g) m.p. 182°-4° C. T.L.C. Silica, ether Rf 0.45.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×40 ml)
  2. customEvaporation of the
  3. washwashed (H2O)
  4. dry with materialdried (MgSO4)
  5. extractionextract
  6. customgave a red oil which
  7. customwas triturated with ether
  8. customcrystallised from ethanol