HRID2259851

反应详情

EQUATION

反应方程式

HRID 2259851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 50.9 g. (0.12 mol) of 2,2'-ethylidenebis(4,6-di-tert-butylphenol) and 1.73 mL (0.018 mol) of 1-methyl-2-pyrrolidinone in 275 mL of toluene at ambient temperature is added dropwise 15.7 mL (0.18 mol) of phosphorus trichloride. After the addition is complete, the reaction mixture is heated at reflux for 18 hours. After cooling to room temperature, the toluene is removed in vacuo and the residue is then recrystallized twice from 250 mL of acetonitrile. The acetonitrile is decanted from the product which is dried under vacuum to give 21.0 g (34.8% yield) of the title compound as an off-white solid melting at 194°-198° C.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturethe reaction mixture is heated
  3. temperatureat reflux for 18 hours
  4. customthe toluene is removed in vacuo
  5. customthe residue is then recrystallized twice from 250 mL of acetonitrile
  6. customThe acetonitrile is decanted from the product which
  7. customis dried under vacuum