反应详情

To a solution of dimethyl 4-methylisophthlate (Chemical Formula 4) (4 g, 19.2 mmol) in distilled dichloromethane were added N-bromosuccinimide (NBS, 4.8 g, 26.9 mmol) and benzoic peroxyanhydride (0.47 g, 19.2 mmol), followed by reaction at 80° C. for 24 hours in a pressure vessel with constant stirring. The reaction progress was monitored by TLC [Hex:EA=3:1]. When the reaction was detected to have reached completion, saturated NaHCO3 was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer thus formed was dried over anhydrous MgSO4, filtered and concentrated in a vacuum. The purification of the concentrate through column chromatography [Hexane: EtOAc=20:1] produced 4 g of dimethyl 4-(bromomethyl)isophthalate (Chemical Formula 5) (70%).

1. customfollowed by reaction at 80° C. for 24 hours in a pressure vessel with constant stirring
2. additionwas added to the reaction mixture
3. extractionfollowed by extraction with dichloromethane
4. customThe organic layer thus formed
5. dry with materialwas dried over anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated in a vacuum
8. customThe purification of the
9. concentrationconcentrate through column chromatography [Hexane: EtOAc=20:1]