HRID2259759

反应详情

EQUATION

反应方程式

HRID 2259759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

62.5 ml of a 1.6 M solution of butyllithium in hexane was added to 500 ml of anhydrous ether. 38.5 g of isopropyltriphenylphosphonium bromide was added thereto in a nitrogen gas stream and the mixture was stirred for 4 h. 18 g of piperonal was added to the reaction mixture and the resulting mixture was stirred for 5.5 h and then filtered. The filtrate was washed with 1 l of ether, concentrated under reduced pressure and purified according to silica gel column chromatography (hexane/ethyl acetate=10:1) to obtain 13.1 g of the intended compound in the form of a colorless oil.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred for 5.5 h
  2. filtrationfiltered
  3. washThe filtrate was washed with 1 l of ether
  4. concentrationconcentrated under reduced pressure
  5. custompurified