HRID1165797

反应详情

EQUATION

反应方程式

HRID 1165797 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.2 g (3.8 mmole) 1,2,3,3a,4,5,6,10c-octahydro-1,3-dioxo-4-phenylpyrrolo[3,4-c]carbazole and 2.2 g (9.7 mmole) DDQ are heated under reflux for 20 hours in 30 ml toluene. 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 of 0.3 is isolated, stirred up with acetone/diisopropyl ether, and the crystals formed are filtered off. One obtains 1,2,3,6-tetrahydro-1,3-dioxo-4-phenyl-pyrrolo[3,4-c]carbazole in the form of yellow crystals of the mp 262°-263° 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 of 0.3 is isolated
  4. customthe crystals formed
  5. filtrationare filtered off