HRID1954761

反应详情

EQUATION

反应方程式

HRID 1954761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of ethyl 4-(4-chloro-2-nitrophenyl)-4- hydroxy-2-butynoate (7.46 g, 26.3 mmoles) in dichloromethane (350 mL) cooled in an ice-bath was added manganese dioxide (26.2 g, 301.3 mmol). The reaction mixture was stirred for 20 minutes and then was allowed to warm to room temperature. The reaction mixture was stirred at room temperature for 130 minutes and then was filtered twice through a pad of CELITE™. The filtrate was purified by flash chromatography on silica gel (195 g), eluting with dichloromethane, to afford 3.80 g (51%) of the title compound as a brownish-orange oil.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at room temperature for 130 minutes
  2. filtrationwas filtered twice through a pad of CELITE™
  3. customThe filtrate was purified by flash chromatography on silica gel (195 g)
  4. washeluting with dichloromethane