HRID2248027

反应详情

EQUATION

反应方程式

HRID 2248027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.11 g (10 mmol) of N-benzylidenebenzylamine N-oxide and 1.64 g (10 mmol) of diethyl vinylphosphonate in 30 ml of toluene under a nitrogen blanket is heated at reflux temperature for 5 days. The solvent is removed under reduced pressure to give 4.45 g of crude product which is then purified by preparative HPLC (Waters Prep 500A, silica gel, 3:2 heptane:ethyl acetate eluent) to give 1.15 g (31% yield) of a caramel-colored liquid.

WORKUP

后处理

  1. temperatureat reflux temperature for 5 days
  2. customThe solvent is removed under reduced pressure
  3. customto give 4.45 g of crude product which
  4. customis then purified by preparative HPLC (Waters Prep 500A, silica gel, 3:2 heptane:ethyl acetate eluent)