HRID1590084

反应详情

EQUATION

反应方程式

HRID 1590084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution was prepared by dissolving 15.7 g of 4,5,7-trichloroquinoline in 60 ml of dry dimethylimidazolidinone. To the solution, 10.4 g of 4,6-dimethyl-2-mercaptopyrimidine was added with stirring at the room temperature. The reaction was progressed with heat evolution and the temperature of the reaction mixture was increased to 50° C. Crystals were precipitated in the course of the reaction. After finishing the addition, stirring was continued for about 2 hours to complete the reaction. The reaction mixture was mixed with 300 ml of water. Precipitated crystals were filtered and recrystallized from acetone to obtain 20.8 g (91.9% yield) of 5,7-dichloro-4-(4,6-dimethyl-2-pyrimidinylthio)quinoline. Melting point was 182.0°-183.2° C.

WORKUP

后处理

  1. customA solution was prepared
  2. temperaturewith heat evolution
  3. temperaturethe temperature of the reaction mixture was increased to 50° C
  4. customCrystals were precipitated in the course of the reaction
  5. additionthe addition
  6. stirringstirring
  7. customthe reaction
  8. customPrecipitated crystals
  9. filtrationwere filtered
  10. customrecrystallized from acetone