反应详情

温度

55 °C

To a stirred solution of [3-(3-chloro-phenyl)-3-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-propyl]-carbamic acid tert-butyl ester (0.15 g, 0.36 mmol) in THF (2 mL) and methanol (2 mL) was added hydrazine hydrate (0.18 g, 3.6 mmol). The mixture was heated at 55° C. for 2 hours. Then the reaction mixture was concentrated and extracted with ethyl acetate (10 mL). The organic mixture was washed with water (3×1 mL), brine (1 mL), dried over anhydrous sodium sulfate and concentrated to dryness. The residue was purified by column chromatography (methanol:dichloromethane, 1:100) to afford [3-amino-3-(3-chloro-phenyl)-propyl]-carbamic acid tert-butyl ester. (Yield 0.061 g, 60%). LC-MS: [M+H]+ 285.

1. concentrationThen the reaction mixture was concentrated
2. extractionextracted with ethyl acetate (10 mL)
3. washThe organic mixture was washed with water (3×1 mL), brine (1 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated to dryness
6. customThe residue was purified by column chromatography (methanol:dichloromethane, 1:100)