反应详情

温度

50 °C

To a solution of 5-(4-{5-[(4-fluorophenyl)methyl]-6-methylpyrimidin-4-yl}-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-3-nitropyridin-2-amine (0.36 g, 0.75 mmol) in acetic acid (10 mL) was added tin (II) chloride (0.75 g, 3.8 mmol). The reaction mixture was heated (50° C.) for 2 h and then partitioned between ethyl acetate (10 mL) and 1 N aqueous sodium hydroxide (20 mL). The resulting mixture was filtered through Celite and the organic layer was washed with brine (10 mL), dried over anhydrous magnesium sulfate then filtered and concentrated. Column chromatography on silica (5% methanol/dichloromethane) provided 5-(4-{5-[(4-fluorophenyl)methyl]-6-methylpyrimidin-4-yl}-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)pyridine-2,3-diamine (0.21 g, 60% yield) as a pale yellow solid. MS (EI) for C26H25FN6O: 457 (MH+).

1. custompartitioned between ethyl acetate (10 mL) and 1 N aqueous sodium hydroxide (20 mL)
2. filtrationThe resulting mixture was filtered through Celite
3. washthe organic layer was washed with brine (10 mL)
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationthen filtered
6. concentrationconcentrated