反应详情

A mixture of 3-bromo-2-methoxyaniline (3 g), 3-carboxyphenylboronic acid (2.94 g), bis(triphenylphosphine)palladium(II)chloride [PdCl2(PPh3)2] (0.30 g) and potassium carbonate (5.2 g) in ethanol (100 mL) and water (20 mL) was heated to about reflux temperature and stirred for about 28 hours. The hot mixture was filtered to remove the catalyst. The clear filtrate was concentrated under vacuum. To the residue, water (50 mL) and methanol (50 mL) was added, acidified to pH 3-5 using hydrochloric acid and stirred for about 30 minutes at about room temperature. The slurry was filtered, washed with n-hexane (50 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours. Yield: 1.8 g

1. temperaturewas heated
2. temperatureto about reflux temperature
3. filtrationThe hot mixture was filtered
4. customto remove the catalyst
5. concentrationThe clear filtrate was concentrated under vacuum
6. additionTo the residue, water (50 mL) and methanol (50 mL) was added
7. stirringstirred for about 30 minutes at about room temperature
8. filtrationThe slurry was filtered
9. washwashed with n-hexane (50 mL)
10. customdried in an oven at about 55° C. to about 60° C. for about 12 hours