反应详情

温度

0 °C

To a stirred solution of 1 g (4.76 mmol) of tert-butyl 3-cyano-4-oxopyrrolidine-1 carboxylate in ethanol (28 mL) was added 0.326 g (4.76 mmol) of hydrazine hydrochloride and the reaction mixture heated at ° C. for 3 h. The mixture was cooled to 0° C. and saturated aqueous sodium hydrogen carbonate (60 mL) added. The solvent was evaporated in vacuo and the aqueous phase extracted with ethyl acetate (10×10 mL). The combined organic fractions were dried (anhydrous sodium sulfate), filtered and the solvent evaporated in vacuo. The resulting residue was chromatographed on a Biotage Horizon® system (silica gel, 0 to 10% methanol/ethyl acetate gradient) to yield the title compound as a orange solid. LC/MS 225.2 (M+1).

1. temperaturethe reaction mixture heated at ° C
2. customThe solvent was evaporated in vacuo
3. extractionthe aqueous phase extracted with ethyl acetate (10×10 mL)
4. dry with materialThe combined organic fractions were dried (anhydrous sodium sulfate)
5. filtrationfiltered
6. customthe solvent evaporated in vacuo
7. customThe resulting residue was chromatographed on a Biotage Horizon® system (silica gel, 0 to 10% methanol/ethyl acetate gradient)