HRID1165794
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- distillationThe solvent is distilled off in a vacuum
- customthe residue chromatographed on silica gel with toluene/ethyl acetate 3:1
- customThe fraction with the Rf 0.3 is isolated
- customrecrystallized from cyclohexane/acetone