反应详情

温度

65 °C

A mixture of 1-[4-chloro-3′-fluoro-5-methyl-6-(1H-tetrazol-5-yl)biphenyl-2-yl]ethanone (85 mg, 0.26 mmol), ammonium acetate (198 mg, 2.57 mmol) and sodium cyanoborohydride (32 mg, 0.51 mmol) in methanol (0.9 mL) and acetonitrile (0.9 mL) was heated at 65° C. overnight in a sealed tube. The mixture was cooled to room temperature and quenched with saturated sodium bicarbonate and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and evaporated to dryness. The crude product was used directly in next step (45 mg, 53%). LCMS calculated for C6H13ClFN4 (M−NH2)+: m/z=315.1. found: 315.1.

1. temperatureThe mixture was cooled to room temperature
2. customquenched with saturated sodium bicarbonate
3. extractionextracted with ethyl acetate
4. dry with materialThe combined extracts were dried over magnesium sulfate
5. customevaporated to dryness