HRID1516204

反应详情

EQUATION

反应方程式

HRID 1516204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 3-chloro-6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazine (2.0 g, 6.6 mmol) in methanol (80 mL) was added sodium carbonate (710 mg, 6.6 mmol), 1,1′-bis(diphenylphosphino)ferrocene (367 mg, 0.6 mmol) and palladium(II) acetate (149 mg, 0.6 mmol). The resulting mixture was stirred at 50° C. overnight under a carbon monoxide atmosphere. After cooling to room temperature it was filtered through Celite® and concentrated. Purification by chromatography (silica, dichloromethane:methanol 1:0 to 9:1) afforded the title compound (960 mg, 40%) as a light brown solid. MS: m/e=326.3 [M+H]+.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature it
  2. filtrationwas filtered through Celite®
  3. concentrationconcentrated
  4. customPurification by chromatography (silica, dichloromethane:methanol 1:0 to 9:1)