HRID4761

反应详情

EQUATION

反应方程式

HRID 4761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a 500 mL round bottom flask there was added 400 mL of dry tetrahydrofuran followed by 0.081 mole of HPPh2. The mixture was cooled to 0° C. and 0.081 mole of n-butyl lithium was slowly added to generate LiPPh2 ; this was slowly warmed to room temperature and stirred for about one hour. The solution was transferred to a dropping funnel and added dropwise to a flask containing 100 mL of 1,3-dichloropropane dissolved in 100 mL of diethyl ether. After stirring overnight the mixture was hydrolyzed with 25 mL of water. The organic layer was separated and the solvent removed by vacuum to leave Ph2P(CH2)3Cl that was stored under nitrogen until needed.

WORKUP

后处理

  1. temperaturethis was slowly warmed to room temperature
  2. customThe solution was transferred to a dropping funnel
  3. additionadded dropwise to a flask
  4. stirringAfter stirring overnight the mixture
  5. customThe organic layer was separated
  6. customthe solvent removed by vacuum