反应详情

温度

80 °C

5.3 mL triethylamine and 2.6 g hydroxylamine hydrochloride were added to 6.8 g 4-cyano-piperazine-1-carboxylic acid tert-butyl ester in 50 mL ethanol. The reaction was stirred 2 h at 80° C. The solvent was removed and 50 mL pyridine and 3.7 mL acetic anhydride were added to the residue and stirred at 80° C. over night. The mixture was evaporated. Water was added and the precipitate was filtered and purified by chromatography on silica gel (cyclohexane/ethyl acetate: 2/1) to give 3.35 g of the desired product.

1. customThe solvent was removed
2. addition50 mL pyridine and 3.7 mL acetic anhydride were added to the residue
3. stirringstirred at 80° C. over night
4. customThe mixture was evaporated
5. additionWater was added
6. filtrationthe precipitate was filtered
7. custompurified by chromatography on silica gel (cyclohexane/ethyl acetate: 2/1)