HRID40748

反应详情

EQUATION

反应方程式

HRID 40748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A mixture of 3,5-dibromobenzonitrile (0.58 g, 2.2 mmol), phenylboronic acid (0.24 g, 2.0 mmol), Pd(PPh3)4 (0.23 g, 0.1 mmol), K2CO3 (3 mL 2 M aqueous solution) and DME (3 mL) was degassed and heated to 95° C. for 12 hr under argon. The reaction mixture was diluted with EtOAc and washed with water. The aqueous layer was extracted with ethyl acetate (2×). The combined organics were dried (MgSO4) and concentrated to give the crude product which was purified with chromatography on silica gel (EtOAc/hexanes) to afford 5-bromobiphenyl-3-carbonitrile.

WORKUP

后处理

  1. customwas degassed
  2. additionThe reaction mixture was diluted with EtOAc
  3. washwashed with water
  4. extractionThe aqueous layer was extracted with ethyl acetate (2×)
  5. dry with materialThe combined organics were dried (MgSO4)
  6. concentrationconcentrated
  7. customto give the crude product which
  8. customwas purified with chromatography on silica gel (EtOAc/hexanes)