HRID1470339

反应详情

EQUATION

反应方程式

HRID 1470339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. customThe solvent is removed in vacuo
  2. customthe product purified over column chromatography (SiO2, heptan, ethyl acetate)