反应详情

温度

100 °C

To a solution of (bromomethylene)dibenzene (115 mg, 1.0 mmol) and piperidin-4-ylmethanol (247 mg, 1.0 mmol) in DMF (5 mL) was added potassium carbonate (276 mg, 2.0 mmol), and the reaction mixture was stirred at 100° C. for 16 h. After cooling to room temperature, the mixture was quenched with water (50 mL) and extracted with ethyl acetate (10 mL×3). The combined organic layers were washed with brine (20 mL), dried over anhydrous sodium sulfate, filtered, and concentrated. The residue was purified by silica column chromatography (eluting with petroleum ether/ethyl acetate=3/1) to give (1-benzhydrylpiperidin-4-yl)methanol (280 mg, 99% yield) as white solid. LCMS (ESI) m/z: 281.9 [M+H]+.

1. temperatureAfter cooling to room temperature
2. customthe mixture was quenched with water (50 mL)
3. extractionextracted with ethyl acetate (10 mL×3)
4. washThe combined organic layers were washed with brine (20 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica column chromatography (eluting with petroleum ether/ethyl acetate=3/1)