HRID5244

反应详情

EQUATION

反应方程式

HRID 5244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 150.2 g. phenyl glycidyl ether (1.0 eq.), 200.0 g. AOnPA (1.15 eq., of Example 1), 200.0 g. toluene, 4.0 g. tetrapropylammonium bromide (0.015 eq.), and 1.0 g. phenothiazine was heated at reflux for 6.0 hours. Conversion, measured by residual oxirane titer, was ca. 93%. Upon cooling, the reactor was charged with 186.0 g. of the AOnPA (1.07 eq.), 150.0 g. toluene, and 10.0 g. p-toluenesulfonic acid monohydrate (0.05 eq.). The mixture was again heated at reflux. After 6.0 hrs., conversion was 90%. The product was extracted with ether and purified by washing. It had an acrylate titer of 3.8 meq./g. (theory: 4.17 meq./g.) and Brookfield viscosity of 230 centipoise at 25° C.

WORKUP

后处理

  1. temperatureat reflux for 6.0 hours
  2. temperatureUpon cooling
  3. additionthe reactor was charged with 186.0 g
  4. temperatureThe mixture was again heated
  5. temperatureat reflux
  6. extractionThe product was extracted with ether
  7. custompurified
  8. washby washing
  9. customat 25° C.