HRID1516204
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling to room temperature it
- filtrationwas filtered through Celite®
- concentrationconcentrated
- customPurification by chromatography (silica, dichloromethane:methanol 1:0 to 9:1)