HRID2169122

反应详情

EQUATION

反应方程式

HRID 2169122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of (2-bromophenyl)-acetonitrile (13) (5 g, 25.51 mmol) in a mixture of toluene and ethanol (1:1, 150 mL) was added 2-chloro phenyl boronic acid (14) (6 g, 38.2 mmol) and Na2CO3 (8.1 g, 76.53 mmol) at room temperature. Purging was conducting for 30 min with nitrogen. Then triphenyl phosphine (2.6 g, 10.2 mmol) was added followed by Pd(OAc)2 (0.287 g, 1.27 mmol) and further degassing was conducted for another 10 min. The reaction mixture was heated to reflux for 10 h. After completion of the reaction, the mixture was concentrated under reduced pressure to get a crude product which was purified using a silica column using 2% ethyl acetate in hexane to get (2′-chloro-biphenyl-2-yl)-acetonitrile (15) (4.9 g, 84.36%) as a yellow liquid.

WORKUP

后处理

  1. customPurging
  2. customfurther degassing
  3. waitwas conducted for another 10 min
  4. temperatureThe reaction mixture was heated
  5. temperatureto reflux for 10 h
  6. customAfter completion of the reaction
  7. concentrationthe mixture was concentrated under reduced pressure
  8. customto get a crude product which
  9. customwas purified