反应详情

温度

60 °C

N-Boc-3-cyano-4-pyrrolidinone (5 g, 23.78 mmol) and hydrazine monohydrochloride (1.629 g, 23.78 mmol) were dissolved in ethanol (140 ml). The mixture was heated to 60° C. for 3 h. The mixture was cooled to 0° C. and saturated aqueous NaHCO3 (50 mL) was added slowly, remaining water was extracted four times with ethyl acetate. The organic phase was dried over Na2SO4 (anhydrous). The residue was purified by column chromatography on silica gel Biotage 40M, eluting with EtOAc/MeOH/aqueous ammonia (gradient from 0 to 10%) to give the title product as a yellow foam. LC-MS: 224.99 (M+1).

1. temperatureThe mixture was cooled to 0° C.
2. extractionwas extracted four times with ethyl acetate
3. dry with materialThe organic phase was dried over Na2SO4 (anhydrous)
4. customThe residue was purified by column chromatography on silica gel Biotage 40M
5. washeluting with EtOAc/MeOH/aqueous ammonia (gradient from 0 to 10%)