HRID2409152

反应详情

EQUATION

反应方程式

HRID 2409152 的结构方程式

PROCEDURE

实验过程

A solution of 3-chloro-6,7-dihydro-5H-cyclopentapyridine 1-oxide (1 g, 5.9 mmole) in acetic anhydride (30 ml) was heated to 110° C. and stirred at this temperature for 20 h. The solvent was evaporated and the residue was partitioned between aqueous saturated NaHCO3 solution and dichloromethane. The organic layer was dried, evaporated and the residue was purified by flash chromatography over silica using EtOAc/n-heptane (gradient from 0% to 30% EtOAc) to give the title compound as a red liquid (880 mg, 71% yield). MS (ESI): m/z=212.0 [M+H]+.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. customthe residue was partitioned between aqueous saturated NaHCO3 solution and dichloromethane
  3. customThe organic layer was dried
  4. customevaporated
  5. customthe residue was purified by flash chromatography over silica