HRID1701264

反应详情

EQUATION

反应方程式

HRID 1701264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,6-Di-tert.-butyl-1,4-benzoquinone (11.0 grams; 0.05 mole) and bis-(2-cyanoethyl)phosphine oxide (8.0 grams; 0.05 mole) are dissolved in 20 mls. of N,N-dimethylacetamide and the solution is heated at reflux for 2 hours. The solution is then cooled to ambient conditions and drowned in water to precipitate a pale yellow oil which is subsequently separated, washed well with water, and extracted with diethyl ether. The ethereal extract is then stripped of diethyl ether and the residue is dried in vacuo at 50° C. to obtain 7.56 grams of a yellow oil which has an infrared absorption spectrum consistent with the desired product.

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. temperatureThe solution is then cooled to ambient conditions
  3. customto precipitate a pale yellow oil which
  4. customis subsequently separated
  5. washwashed well with water
  6. extractionextracted with diethyl ether
  7. extractionThe ethereal extract
  8. customthe residue is dried in vacuo at 50° C.