反应详情

To a round bottomed flask was added NaHCO3 (22.31 g, 266 mmol), 5-chloro-2-iodobenzoic acid (25 g, 89 mmol), DMF, and MeI (11.07 mL, 177 mmol). The reaction was stirred at room temperature overnight. The reaction was diluted with water and EtOAc. The layers were separated and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with water (3×) and brine before being dried over Na2SO4, filtered, and concentrated. The crude residue was purified via Biotage to afford the titled compound (25.81 g, 87 mmol). LC/MS m/z 297 [M+H]+.

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with EtOAc
3. washThe combined organic layers were washed with water (3×) and brine
4. dry with materialbefore being dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude residue was purified via Biotage