HRID569654

反应详情

EQUATION

反应方程式

HRID 569654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

26.3 g (0.12 mol) of 8-chloro-1,2,3,4,5,6-hexahydrobenzo[f]quinoline dissolved in 3 l of methylene chloride were added to a solution of 4.75 g (0.03 mol) of potassium permanganate and 514 g (2.4 mol) of sodium periodate in 12 l of water, 3.00 g (0.013 mol) of benzyltriethylammonium chloride were added thereto and the mixture was stirred at room temperature overnight. The mixture was filtered over Dicalit and extracted with methylene chloride. Drying with sodium sulphate, distillation of the solvent in vacuo and chromatography (silica gel, ethyl acetate) gave 11-chloro-1,2,4,5,6,7-hexahydro-4-benzazecine-3,8-dione as beige crystals of melting point 142°-144°.

WORKUP

后处理

  1. additionwere added
  2. filtrationThe mixture was filtered over Dicalit
  3. extractionextracted with methylene chloride
  4. dry with materialDrying with sodium sulphate, distillation of the solvent in vacuo and chromatography (silica gel, ethyl acetate)