HRID1675243

反应详情

EQUATION

反应方程式

HRID 1675243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

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 and then aqueous Na2CO3 (39 mL, 20% by weight) was added. The resulting mixture was heated at 70° C. for 4 hours. The precipitate was filtered and rinsed with a 20% aqueous Na2CO3 solution. The filtrate was diluted with water and acidified to a pH of 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

WORKUP

后处理

  1. filtrationThe precipitate was filtered
  2. washrinsed with a 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