HRID630501

反应详情

EQUATION

反应方程式

HRID 630501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Potassium carbonate (1.16 g, 8.45 mmol) and bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (0.2 g, 0.28 mmol) were added under an argon atmosphere and at room temperature to a solution of 223b) (1.5 g, 2.8 mmol) and phenyl boronic acid (0.69 g, 5.63 mmol) in tert-butanol/water (10:1, 66 mL). The resulting mixture was heated at 90° C. for 2 h, then cooled to room temperature and filtered through a pad of celite. The filtrate was concentrated and the remnant purified by flash column chromatography [silica gel, dichloromethane with 2% methanol] and then triturated with ether. White solid. Yield: 1 g (67% of theory)

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationfiltered through a pad of celite
  3. concentrationThe filtrate was concentrated
  4. customthe remnant purified by flash column chromatography [silica gel, dichloromethane with 2% methanol]
  5. customtriturated with ether