反应详情

To a solution of 4,4,4-trifluoro-1-(pyridin-2-yl)butane-1,3-dione (1.0 g, 4.6 mmol) in ethanol (10 mL) was added 2-methyl-2-thiopseudourea sulfate (0.64 g, 4.6 mmol), followed by sodium ethoxide (3.0 mL of 21 wt. % solution in ethanol, 9 mmol). The mixture was heated at reflux for 9 h, then cooled to room temperature and extracted with EA. The EA was washed with water and the solvent removed under reduced pressure. The crude product was purified by column chromatography, eluting with 49:1 chloroform/MeOH, to give 4-trifluoromethyl-2-methylthio-6-(pyridin-2-yl)pyrimidine (0.21 g, 17% yield) as an off-white solid.

1. temperatureThe mixture was heated
2. temperatureat reflux for 9 h
3. extractionextracted with EA
4. washThe EA was washed with water
5. customthe solvent removed under reduced pressure
6. customThe crude product was purified by column chromatography
7. washeluting with 49:1 chloroform/MeOH