HRID1450028

反应详情

EQUATION

反应方程式

HRID 1450028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
-80 °C

PROCEDURE

实验过程

52 ml (83.2 mmols) of a 1.6M n-butyllithium solution in hexane are added to a suspension, cooled to -10° C., of 34 g (85.1 mmols) of n-butyltriphenylphosphonium bromide in 150 ml of tetrahydrofuran. After 20 minutes' reaction, the whole is cooled to -80° C. and 50 ml of hexamethylphosphoric triamide are added, as well as 10 g (54 mmols) of 4-bromobenzaldehyde dissolved in 40 ml of tetrahydrofuran. After returning to room temperature and hydrolysis with a saturated ammonium chloride solution, the reaction mixture is extracted with ether. Customary treatment of the organic phase yields 10 g of the expected compound after purification by chromatography on a silica column (eluent: petroleum ether).

WORKUP

后处理

  1. customAfter 20 minutes' reaction
  2. customAfter returning to room temperature
  3. extractionthe reaction mixture is extracted with ether