反应详情

温度

40 °C

3',4',5'-Trimethoxyacetophenone (15.0 g) and pyrrolidone hydrotribromide (35.39 g) were dissolved in tetrahydrofuran (225 ml), followed by stirring at 40° C. for one hour. The reaction solution was cooled to room temperature, precipitated crystals were filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography, and the obtained crude crystals were washed with hexane (100 ml) to give 2-bromo-3',4',5'-trimethoxyacetophenone (Compound XIa, 12.20 g).

1. temperatureThe reaction solution was cooled to room temperature
2. customprecipitated crystals
3. filtrationwere filtered off
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography
6. customthe obtained crude crystals
7. washwere washed with hexane (100 ml)