HRID979526

反应详情

EQUATION

反应方程式

HRID 979526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2,3-dimethyl-6-nitrobenzenemethanol (34.88 g, 0.192 mole) in dichloromethane (150 mL) was added to a stirred mixture of pyridinium chlorochromate (62.2 g, 0.288 mole) in dichloromethane (250 ml). The mixture was stirred vigorously for 4 hours, diluted with diethyl ether (500 mL) and the organic layer decanted. The residue was washed with diethyl ether (500 mL) and the combined organic solution filtered through a plug of silica gel (6"×11/2"). Evaporation of the solvent afforded 2,3-dimethyl-6-nitrobenzaldehyde (32.08 g, 93%). An analytical sample was prepared by crystallizing from diisopropyl ether and had m.p. 66°-68° C.

WORKUP

后处理

  1. customthe organic layer decanted
  2. washThe residue was washed with diethyl ether (500 mL)
  3. filtrationthe combined organic solution filtered through a plug of silica gel (6"×11/2")
  4. customEvaporation of the solvent