反应详情

温度

65 °C

A mixture of 1-(4-chloro-3′-fluoro-5-methyl-6-nitrobiphenyl-2-yl)ethanone (50 mg, 0.2 mmol) and ammonium acetate (130 mg, 1.7 mmol) in methanol (1 mL) and acetonitrile (1 mL) was heated at 65° C., in a sealed tube, for 30 min. The mixture was cooled to room temperature and sodium cyanoborohydride (22 mg, 0.35 mmol) was added. The reaction was heated at 65° C. for another 4 hours, cooled to room temperature, quenched with saturated sodium bicarbonate, and extracted with dichloromethane. The combined extracts were dried over magnesium sulfate and evaporated to dryness. The residue was used directly in next step. LCMS calculated for C15H15ClFN2O2 (M+H)+: m/z=309.1. found: 309.1.

1. temperatureThe mixture was cooled to room temperature
2. temperatureThe reaction was heated at 65° C. for another 4 hours
3. temperaturecooled to room temperature
4. customquenched with saturated sodium bicarbonate
5. extractionextracted with dichloromethane
6. dry with materialThe combined extracts were dried over magnesium sulfate
7. customevaporated to dryness