反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
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 5-bromo-2-(4-(methoxymethoxy)phenyl)-3-nitropyridine (68 mg, 0.2 mmol), 2-fluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (45 mg, 0.2 mg), tetrakis(triphenylphosphine)palladium (12 mg, 0.01 mmol), Na2CO3 (0.5 mL, 1 M aqueous solution) and dioxane (1.5 mL) was heated at 100° C. for 10 min in a microwave reactor. After cooling to rt, the reaction was diluted with EtOAc (20 mL) and washed with brine (20 mL) and water (2×20 mL) and dried over MgSO4. Solvent was removed under reduced pressure and the residue was purified by silica chromatography (EtOAc in hexane, 5% to 40%) to afford 6′-fluoro-6-(4-(methoxymethoxy)phenyl)-5-nitro-3,3′-bipyridine as a yellow solid (48 mg, 67%). MS (ESI) m/z [M+H]+356.
WORKUP
后处理
- temperatureAfter cooling to rt
- washwashed with brine (20 mL) and water (2×20 mL)
- dry with materialdried over MgSO4
- customSolvent was removed under reduced pressure
- customthe residue was purified by silica chromatography (EtOAc in hexane, 5% to 40%)