反应详情

温度

50 °C

tert-Butyl (Z)-4-[4-(methoxycarbonyl)-2-(prop-1-en-1-yl)phenyl]piperazine-1-carboxylate (96 mg, 0.267 mmol) was dissolved in methanol (3.0 mL). Under ice-cold conditions, 4N aqueous solution of sodium hydroxide (334 μL) was added, and the mixture was stirred at 50° C. overnight. Subsequently, 4N aqueous solution of sodium hydroxide (668 μL) was further added under ice-cold conditions, and stirred at 50° C. overnight. The reaction solution was added 4N aqueous solution of hydrochloric acid under ice-cold conditions, and extracted with chloroform. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/acetone). The title compound (108 mg (yield >99%)) was obtained as a white crystal.

1. stirringstirred at 50° C. overnight
2. extractionextracted with chloroform
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe obtained residue was purified by silica-gel column chromatography (hexane/acetone)