反应详情

Phosphorous oxychloride (26.11 g, 170 mmol) was added to dimethylformamide (180 ml) and stirred 20 min. 2-mercapto-3-methyl-6-(4-pyridyl)-pyrimidine-4-one (24.15 g, 110 mmol) was added to the solution and stirred 5 min and then stirred at 70° C. for 2 hours. Ethyl acetate (630 ml) was added to the ice-cooled solution and precipitate was collected by filtration after 20 minutes stirring. After drying, the precipitate was dissolved in water (400 ml) and pH was adjusted to 10 by aqueous sodium hydroxide. The precipitate was washed with water, filtered and dried to give the title compound (18.82 g, 77%).

1. stirringstirred 5 min
2. stirringstirred at 70° C. for 2 hours
3. temperaturecooled solution and precipitate
4. filtrationwas collected by filtration after 20 minutes
5. stirringstirring
6. customAfter drying
7. dissolutionthe precipitate was dissolved in water (400 ml)
8. washThe precipitate was washed with water
9. filtrationfiltered
10. customdried