HRID2268490

反应详情

EQUATION

反应方程式

HRID 2268490 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of lithium aluminum hydride (2.37 g) in diethyl ether (150 ml) was dropwise added a solution of 2,3,4,5-tetramethoxy-6-methylbenzaldehyde (15.0 g) in diethyl ether (30 ml) with cooling with ice. After the reaction mixture was stirred for 30 min, 10% hydrochloric acid was added to the reaction mixture, which was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (hexane to hexane:ethyl acetate=2:1) to yield the entitled compound (14.2 g) as an oil.

WORKUP

后处理

  1. temperaturewith cooling with ice
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated aqueous sodium chloride
  4. customdried
  5. customThe solvent was removed in vacuo
  6. customThe residue was purified by silica gel column chromatography (hexane to hexane:ethyl acetate=2:1)