反应详情

5-Bromo-2-fluoropyridin-3-ylboronic acid (14.87 g, 67.7 mmol) (Frontier Scientific) and 2,2′-(methylazanediyl)diacetic acid (10.95 g, 74.4 mmol) (Aldrich) were dissolved in toluene (242 mL) and DMSO (97 mL) and the resulting mixture was heated at reflux under a Dean Stark trap for 2 h. After water (>2.5 mL) was collected in the trap, the reaction mixture was concentrated in vacuo to remove toluene, and water was slowly added to the resulting solution until the desired product precipitated as a white solid. This solid was collected by vacuum filteration, washed with water, and dried in a vacuum oven to give the title compound (82% yield) as a fluffy white solid. m/z (ESI, +ve ion) 330.8/332.9 (M+H)+.

1. temperatureat reflux under a Dean Stark trap for 2 h
2. customAfter water (>2.5 mL) was collected in the trap
3. concentrationthe reaction mixture was concentrated in vacuo
4. customto remove toluene, and water
5. additionwas slowly added to the resulting solution until the desired product
6. customprecipitated as a white solid
7. customThis solid was collected by vacuum filteration
8. washwashed with water
9. customdried in a vacuum oven