HRID711234
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
- 100 °C
PROCEDURE
实验过程
A mixture of (2-fluoropyridin-4-yl)boronic acid 24-1 (200 mg, 1.42 mmol), (6-chloropyridin-3-yl)methanamine 18-1 (142 mg, 1.00 mmol), Pd(OAc)2 (12 mg, 0.05 mmol), dicyclohexyl(2′,6′-dimethoxy-[1,1′-biphenyl]-2-yl)phosphine (41 mg, 0.1 mmol) and K3PO4 (424 mg, 2.00 mmol) in 2-butanol (1 mL) was stirred at 100° C. under argon overnight. After cooling to room temperature, the mixture was filtered through celite (washed with ethyl acetate), concentrated by rotavap and the residue subjected to silica gel column chromatography with 7% ammonia-saturated methanol in dichloromethane as eluent to give (2′-fluoro-[2,4′-bipyridin]-5-yl)methanamine 24-2 as an oil.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe mixture was filtered through celite (washed with ethyl acetate)
- concentrationconcentrated by rotavap