反应详情

To a solution of N-{2-[(3-bromophenyl)carbonyl]-4,5-dimethoxyphenyl}-2,2-dimethylpropanamide (7.9 g, 18.9 mmol) in 1,4-dioxane (80 mL) was added concentrated HCl (9.55 g, 94.2 mmol). The mixture was refluxed for 2 hours. After cooling to room temperature, 1,4-dioxane was removed in vacuum and the residue was diluted with water (100 mL) and EtOAc (100 mL), then neutralized with NaHCO3 to pH=8. The mixture was extracted with EtOAc (80 mL×3). The combined organic phases were dried over anhydrous MgSO4, filtered and concentrated under vacuum to afford (2-amino-4,5-dimethoxyphenyl)(3-bromophenyl)methanone. MS (M+H)=336 and 338.

1. temperatureThe mixture was refluxed for 2 hours
2. custom1,4-dioxane was removed in vacuum
3. additionthe residue was diluted with water (100 mL) and EtOAc (100 mL)
4. extractionThe mixture was extracted with EtOAc (80 mL×3)
5. dry with materialThe combined organic phases were dried over anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum