反应详情

After dissolving 2-[5-bromo-3-(dimethylamino)-2-methoxyphenyl]-2-propanol (410 mg) in 100 mL of methanol-hydrochloric acid, the solution was heated to reflux for 14 hours. The reaction mixture was cooled to room temperature, saturated aqueous sodium hydrogencarbonate was added for neutralization, water was added and extraction was performed with ethyl acetate. The organic layer was washed with brine and then dried over anhydrous magnesium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (370 mg) as an oil. 1H-NMR (CDCl3) δ: 1.57(3H, s), 1.60(3H, s), 2.77(6H, s), 3.40(3H, s), 3.77(3H, s), 6.95(1H, d, J=2 Hz), 7.16(1H, d, J=2 Hz).

1. temperaturethe solution was heated
2. temperatureto reflux for 14 hours
3. additionwas added
4. extractionextraction
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationAfter distilling off the solvent under reduced pressure
8. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)