反应详情

温度

65 °C

A mixture of 1-{5-chloro-8-[(3S)-3-fluoropyrrolidin-l-yl]quinolin-7-yl}ethanone (0.10 g, 0.34 mmol) and ammonium acetate (0.263 g, 3.42 mmol) in methanol (1.5 mL) and acetonitrile (1.5 mL) was heated at 65° C. in a sealed tube for 1 hour. After cooling to room temperature, sodium cyanoborohydride (0.064 g, 1.0 mmol). The reaction was heated at 65° C. overnight, cooled to room temperature and quenched with sat. NaHCO3 solution and extracted with Ethyl acetate. The combined organic layers were dried over MgSO4, concentrated and purified on a preparative LCMS (pH=10) to give the desired product. LCMS calculated for C15H18ClFN3 (M+H)+: m/z=294.1; Found: 294.0.

1. temperatureAfter cooling to room temperature
2. temperatureThe reaction was heated at 65° C. overnight
3. temperaturecooled to room temperature
4. customquenched with sat. NaHCO3 solution
5. extractionextracted with Ethyl acetate
6. dry with materialThe combined organic layers were dried over MgSO4
7. concentrationconcentrated
8. custompurified on a preparative LCMS (pH=10)