反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customA solution was prepared
- temperaturewith heat evolution
- temperaturethe temperature of the reaction mixture was increased to 50° C
- customCrystals were precipitated in the course of the reaction
- additionthe addition
- stirringstirring
- customthe reaction
- customPrecipitated crystals
- filtrationwere filtered
- customrecrystallized from acetone