HRID399272

反应详情

EQUATION

反应方程式

HRID 399272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A stirred solution of 4-bromo-3-methylbenzonitrile (5.0 g, 0.026 mole) and 4-boronobenzoic acid (4.2 g, 0.026 mole) in a mixture of DME (100 ml) and water (100 ml) under argon was treated with sodium carbonate (11.6 g, 0.11 mole) and tetrakis (triphenylphosphine) palladium (O) (0.55 g) and heated under reflux for 20 h. The solution was concentrated in vacuo to approx. 100 ml volume, then washed with ethyl acetate and acidified with 5M HCl acid. The solid which was produced was filtered off, washed with water and dried in vacuo to afford the title compound as a white solid (4.16 g, 69%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 20 h
  3. concentrationThe solution was concentrated in vacuo to approx. 100 ml volume
  4. washwashed with ethyl acetate
  5. customThe solid which was produced
  6. filtrationwas filtered off
  7. washwashed with water
  8. customdried in vacuo