HRID329526

反应详情

EQUATION

反应方程式

HRID 329526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 20.37 g of 7-(tetrahydropyran-2-yloxy)-1-heptanol in 200 ml of methylene chloride was added, whilst ice-cooling, to a mixture of 40.60 g of pyridinium chlorochromate, 3.86 g of sodium acetate and 200 ml of methylene chloride. The resulting mixture was stirred at 0° C. for 1 hour and then at room temperature for 3 hours, after which was diluted with 1.5 liter of diethyl ether and passed through a column containing 250 g of silica gel. The eluate was concentrated by evaporation under reduced pressure, and the residue was subjected to column chromatography through 400 g of silica gel. 14.11 g of 7-(tetrahydropyran-2-yloxy)heptanal were obtained, as a colorless oil, from those fractions eluted with mixtures of hexane and ethyl acetate ranging from 40:1 to 9:1 by volume.

WORKUP

后处理

  1. waitat room temperature for 3 hours
  2. additioncontaining 250 g of silica gel
  3. concentrationThe eluate was concentrated by evaporation under reduced pressure