HRID548874
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 (6-iodo-pyridazine-3-yl)-(5-methyl-3-phenyl-isoxazol-4ylmethyl)-amine (1.0 g, 2.6 mmol) in methanol (3 mL) was added sodium carbonate (270 mg, 2.6 mmol), 1,1′-bis(diphenylphosphino)ferrocene (141 mg, 0.26 mmol) and palladium(II) acetate (57 mg, 0.26 mmol). The resulting mixture was heated at 50° C. for 16 h under a carbon monoxide atmosphere. After cooling to room temperature it was filtered through Celite® and concentrated. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 20:80) afforded the title compound (720 mg, 87%) as a light brown solid. MS: m/e=325.3 [M+H]+.
WORKUP
后处理
- temperatureAfter cooling to room temperature it
- filtrationwas filtered through Celite®
- concentrationconcentrated
- customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 20:80)