HRID632060

反应详情

EQUATION

反应方程式

HRID 632060 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Under nitrogen atmosphere, 6-bromo-5-chloro-pyridine-2-carboxylic acid (0.38 g, 1.6 mmol), 3-chlorophenylboronic acid (CAN 63503-60-6, 0.33 g, 2.1 mmol), 1,1′-bis(diphenylphosphino)-ferrocene-palladium(II) dichloride methylene chloride complex (CAN 95464-05-4, 30 mg) and cesium carbonate (CAN 534-17-8, 1.6 g, 4.8 mmol) was added into DMF (30 mL). The mixture was stirred at 80° C. overnight. After evaporation of solvents, the crude product was purified by column chromatography (silica gel, 12 g, petroleum ether/ethyl acetate 4/1 firstly, then methanol/methylene chloride 1/10) to give the title compound (0.14 g, 32%) as brown solid; MS (EI): m/e=268.0 [M+H]+.

WORKUP

后处理

  1. customAfter evaporation of solvents
  2. customthe crude product was purified by column chromatography (silica gel, 12 g, petroleum ether/ethyl acetate 4/1 firstly