反应详情

温度

150 °C

To 4-[(5-bromo-3-methoxy-pyrazin-2-ylamino)-methyl]-piperidine-1-carboxylic acid tert-butyl ester (0.5 g, 0.00125 mol) in DMSO (10 mL), under nitrogen, was added copper cyanide (0.565 g, 0.00625 mol) and the mixture heated to 150° C. for 1.5 h. The reaction mixture was cooled to rt, diluted with a mixture of 20% ammonium hydroxide in water (50 mL) and dichloromethane (50 mL) and allowed to stir for 1 h. The organic layer was removed, dried over sodium sulfate, filtered and concentrated to an oil. The oil was chromatographed on silica using a gradient of 20–40% ethyl acetate/hexane to give the title compound as a foam. M.S.(M+1): 348.

1. temperatureThe reaction mixture was cooled to rt
2. customThe organic layer was removed
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated to an oil
6. customThe oil was chromatographed on silica using a gradient of 20–40% ethyl acetate/hexane