反应详情

温度

35 °C

To a mixed solution of 3.0 g of an iron powder, 15 ml of acetic acid and 1.5 ml of water was added a solution of 3.0 g of 6-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-benzyloxy-3-nitropyridine in 10 ml of acetic acid and 10 ml of ethyl acetate dropwise while maintaining the temperature of the reaction solution at 35° C. or lower. After completion of the addition, the mixture was stirred over night, then, the reaction solution was filtrated through Celite, and the solvent was removed at reduced pressure. The residue was diluted with saturated aqueous sodium bicarbonate solution, extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The resulted residue was subjected to silica gel chromatography to obtain 2.55 g of 3-amino-6-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-benzyloxypyridine

1. additionAfter completion of the addition
2. filtrationthe reaction solution was filtrated through Celite
3. customthe solvent was removed at reduced pressure
4. additionThe residue was diluted with saturated aqueous sodium bicarbonate solution
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with saturated saline
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated