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
- 150 °C
PROCEDURE
实验过程
7-Chloro-2-(3,4,5-trimethoxy-phenyl)-furo[3,2-b]pyridine (0.061 mmol), phenyl boronic acid (0.064 mmol), palladium(II)-acetate (0.004 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (0.006 mmol) and K2CO3 (0.181 mmol) are suspended in 1,4-dioxane (1.00 ml) and water (100.00 μl). The suspension is heated to 150° C. in the microwave for 45 min. The solvent is removed in vacuo and the product purified over column chromatography (SiO2, heptan, ethyl acetate). The product is isolated as yellow solid (yield 32%); HPLC (method A): Rt 2.6 min (purity 93.2%); LCMS (ESI+) (method E): Rt 2.416 min, M+H+ 362.1 m/z; 1H NMR (500 MHz, DMSO-d6) δ [ppm] 8.57 (d, J=5.1, 1H), 8.16-8.10 (m, 2H), 7.74 (s, 1H), 7.65 (t, J=7.7, 2H), 7.60 (d, J=5.1, 1H), 7.56 (t, J=7.4, 1H), 7.31 (s, 2H), 3.91 (s, 6H), 3.74 (s, 3H).
WORKUP
后处理
- customThe solvent is removed in vacuo
- customthe product purified over column chromatography (SiO2, heptan, ethyl acetate)