反应详情

温度

90 °C

To a solution of tert-butyl 1,4-diazepane-1-carboxylate (4.65 g, 23.2 mmol) and 4-chloro-3-hydroxybutanenitrile (2.0 g, 17 mmol) in ethanol (40 mL) was added sodium bicarbonate (2.1 g, 25 mmol). The mixture was stirred at 90° C. for 19 hours. After cooling to room temperature, ethanol was evaporated. The remaining mixture was diluted with ethyl acetate and washed with water and brine. The organic was dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel column (0% to 10% methanol/DCM) to give the desired product as yellow oil (3.2 g, 68%). LCMS calculated for C14H26N3O3(M+H)+: m/z=284.1.

1. temperatureAfter cooling to room temperature
2. customethanol was evaporated
3. additionThe remaining mixture was diluted with ethyl acetate
4. washwashed with water and brine
5. dry with materialThe organic was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica gel column (0% to 10% methanol/DCM)