HRID365039

反应详情

EQUATION

反应方程式

HRID 365039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A magnetically stirred suspension of 1-bromononane (Aldrich, 40 g, 0.1931M) and triphenylphosphine (101.3 g, 0.3862 mole) was heated at 100° C. (oil bath) for 2 hours. The resulting homogeneous solution was then cooled and triturated with ether (8X) to remove most of the unreacted triphenylphosphine. A viscous gum was obtained which was dissolved in CH2Cl2 and concentrated in vacuo to give the title phosphonium salt as a light yellow, extremely hygroscopic foam weighing 85 g (80.1%). TLC, neat CH2Cl2, Rf =0.78, PMA.

WORKUP

后处理

  1. temperatureThe resulting homogeneous solution was then cooled
  2. customtriturated with ether (8X)
  3. customto remove most of the unreacted triphenylphosphine
  4. customA viscous gum was obtained which
  5. concentrationconcentrated in vacuo