反应详情

To a solution of 1.0 g of crude methyl [2-(5-{3,3-dihydroxy-4,4,4-trifluorobutyryl}amino-2-chloro-4-fluorophenoxy)phenoxy]acetate and 3 ml of tetrahydrofuran were added 4 ml of acetic acid and 0.87 g of potassium cyanate, and the mixture was stirred at room temperature for 6 hours and then heated at reflux at 120° C. for 2 hours. After cooling, 30 ml of water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate solution, water and saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.67 g of methyl [2-{2-chloro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]-4-fluorophenoxy}phenoxy]acetate.

1. temperatureheated
2. temperatureat reflux at 120° C. for 2 hours
3. temperatureAfter cooling
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution, water and saturated aqueous sodium chloride solution
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure