反应详情

温度

0 °C

1-[5-(1-Methylethoxy)pyridin-2-yl]ethanol (22 mg, 0.119 mmol) was dissolved in acetone (1.2 mL). The resultant mixture was added with 2,2,6,6-tetramethylpiperidine 1-oxyl (2.0 mg, 0.012 mmol) and trichloroisocyanuric acid (30 mg, 0.131 mmol) under ice-cold conditions, and stirred at 0° C. for 10 minutes. The reaction solution was concentrated in vacuo, added with an aqueous solution of sodium hydrogen carbonate, and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and concentrated in vacuo. The obtained residue was purified using silica-gel column chromatography (hexane/ethyl acetate) and 1-[5-(1-methylethoxy)pyridin-2-yl]ethanone (20 mg, yield 94%) was obtained as a yellow oil.

1. concentrationThe reaction solution was concentrated in vacuo
2. additionadded with an aqueous solution of sodium hydrogen carbonate
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe obtained residue was purified