反应详情

温度

45 °C

To a mixture of 0.55 g of an iron powder, 3 ml of acetic acid and 0.3 ml of water was added a solution of 0.548 g of 4-benzyloxy-3-{4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]-2-nitrophenoxy}pyridine in 0.5 ml of acetic acid and 3 ml of ethyl acetate dropwise. After completion of the addition, the mixture was stirred for 3 hour at 40-50° C. The mixture was poured into water, then, the mixture was filtrated through Celite, and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate solution, and saturated saline, dried over anhydrous magnesium sulfate, and concentrated to obtain 0.438 g of 3-{2-amino-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-4-benzyloxypyridine.

1. additionAfter completion of the addition
2. filtrationthe mixture was filtrated through Celite
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution, and saturated saline
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated