HRID1248231

反应详情

EQUATION

反应方程式

HRID 1248231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 15 parts of 3-(2-hydroxyethyl)-2-phenyl-4-(3H)-quinazolinone and 375 parts of trichloromethane are added dropwise 24 parts of thionyl chloride at room temperature. Upon completion, stirring is continued for 2 hours at reflux. The reaction mixture is evaporated. Water is added to the residue and the whole is neutralized with a sodium hydrogen carbonate solution. The product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The residue is crystallized from a mixture of 2,2'-oxybispropane and petroleumether. The product is filtered off and dried, yielding 11.6 parts of 3-(2-chloroethyl)-2-phenyl-4(3H)-quinazolinone.

WORKUP

后处理

  1. temperatureat reflux
  2. customThe reaction mixture is evaporated
  3. additionWater is added to the residue
  4. extractionThe product is extracted with trichloromethane
  5. washThe extract is washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is crystallized from a mixture of 2,2'-oxybispropane and petroleumether
  10. filtrationThe product is filtered off
  11. customdried