反应详情

温度

80 °C

218.7 g (1.4 mols) of 2-methylthio-4-hydroxy-6-methylpyrimidine are suspended in 1.12 litres of dioxane, and 1500 g (11.2 mols) of 30% aqueous sodium hydroxide solution are added. The suspension is heated to 80° C., and into this hot suspension are passed, in the course of 3 hours, 242 g (2.8 mols) of difluorochloromethane. The pale yellow suspension obtained is cooled to 20° C. and filtered. The residue is washed with dioxane and dried to thus yield 210 g of 2-methylthio-4-difluoromethoxy-6-methylpyrimidine. The filtrate is extracted with methylene chloride, and the organic phase is washed with water and concentrated by evaporation to obtain, as crystalline residue, a further 79 g of the desired product. The overall yield obtained in this manner is 289 g of 2-methylthio-4-difluoromethoxy-6-methylpyrimidine (100% of theory), m.p. 40-42° C.

1. customThe pale yellow suspension obtained
2. temperatureis cooled to 20° C.
3. filtrationfiltered
4. washThe residue is washed with dioxane
5. dry with materialdried to thus yield 210 g of 2-methylthio-4-difluoromethoxy-6-methylpyrimidine
6. extractionThe filtrate is extracted with methylene chloride
7. washthe organic phase is washed with water
8. concentrationconcentrated by evaporation
9. customto obtain, as crystalline residue