HRID1165794

反应详情

EQUATION

反应方程式

HRID 1165794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.5 g (10.2 mmole) 1,3-dihydro-4-(2-nitrophenyl)-1,3-dioxo-7-phenyl-2H-isoindole and 9.5 g (36.2 mmole) triphenylphosphine are heated under reflux for 16 hours in 100 ml 2,4,6-collidine. The solvent is distilled off in a vacuum and the residue chromatographed on silica gel with toluene/ethyl acetate 3:1. The fraction with the Rf 0.3 is isolated and recrystallized from cyclohexane/acetone. One obtains 1,2,3,6-tetrahydro-1,3-dioxo-4-phenylpyrrolo[3,4-c]carbazole in the form of yellow crystals of the mp 262°-264° C.

WORKUP

后处理

  1. distillationThe solvent is distilled off in a vacuum
  2. customthe residue chromatographed on silica gel with toluene/ethyl acetate 3:1
  3. customThe fraction with the Rf 0.3 is isolated
  4. customrecrystallized from cyclohexane/acetone