反应详情

温度

70 °C

To a mixture of 0.18 g of 3-hydroxy-2-{1-(methoxycarbonyl)ethoxy}pyridine, 0.19 g of 2,5-difluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene and 2.0 ml of N,N-dimethylformamide was added 91 mg of potassium carbonate, and the mixture was stirred for 3 hours at 70° C. The reaction solution was cooled to room temperature, then, poured into ice water, and extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.21 g of 3-{4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]-2-nitrophenoxy}-2-{1-(methoxycarbonyl)ethoxy}pyridine [present compound 9-42] (as a mixture of two diastereomerical isomers).

1. temperatureThe reaction solution was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated saline
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated