反应详情

温度

70 °C

The Suzuki coupling was carried out according to the method of Dyer et al. (2001) Tetrahedron Letters 42: 1765-1767. Commercially available 4-(Trifluoromethyl)phenylboronic acid (15 g, 78.7 mmol) and 3-bromobenzoic acid (15.1 g, 75 mmol) were suspended in 2-propanol:water (1:4, 72 mL). 10% Pd/C (1.5 g) was added followed by aqueous Na2CO3 (39 mL, 20% by wt.). The resulting mixture was heated at 70° C. for 4 hours. The precipitate was filtered and rinsed with 20% aqueous Na2CO3 solution. The filtrate was diluted with water and acidified to pH=2. The white solid was filtered and dried in vacuo. The crude material (2.1) (19.69 g) was used in the next step without further purification.

1. filtrationThe precipitate was filtered
2. washrinsed with 20% aqueous Na2CO3 solution
3. additionThe filtrate was diluted with water
4. filtrationThe white solid was filtered
5. customdried in vacuo
6. customThe crude material (2.1) (19.69 g) was used in the next step without further purification