反应详情

A solution of 4-chloro-2-methoxybenzamide (0.74 g, 3.99 mmol) in dichloromethane (50 ml) was cooled to −78° C. followed by addition of BBr3 (1.15 ml, 11.96 mmol) under nitrogen atmosphere. The reaction mixture was allowed to stir at room temperature for 2 h. After the completion of reaction (TLC monitoring), the solution was cooled to 0° C. and quenched with water. The resulting solution was basified by aqueous NaHCO3 and extracted with EtOAc (3×100 ml). The combined organics was dried over anhydrous Na2SO4, filtered and concentrated to get the desired product (0.608 g, 89%). MS: 172.33 (M+H)+.

1. customAfter the completion of reaction (TLC monitoring)
2. temperaturethe solution was cooled to 0° C.
3. customquenched with water
4. extractionextracted with EtOAc (3×100 ml)
5. dry with materialThe combined organics was dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated