反应详情

温度

130 °C

A mixture of 0.776 g 1-methyl-6-trifluoromethyl-2,4-(1H,3H)-pyrimidin-dione, 0.760 g potassium carbonate and 0.768 g 2,6-dichloro-3-fluoro-5-cyanopyridin in 40 ml dimethylsulfoxide is stirred under nitrogen at 130° C. until conversion is complete. Then the reaction mixture is cooled down and diluted with ice and water. The pH of the mixture is adjusted to neutral and the mixture is extracted several times with ethyl acetate. The organic layers are washed with water, dried, evaporated and the residue is purified by silicagel chromatography (hexane/ethyl acetate 7/3) to yield the title compound as a solid of m.p. 146-148° C.

1. temperatureThen the reaction mixture is cooled down
2. extractionis extracted several times with ethyl acetate
3. washThe organic layers are washed with water
4. customdried
5. customevaporated
6. customthe residue is purified by silicagel chromatography (hexane/ethyl acetate 7/3)