HRID593276
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
PROCEDURE
实验过程
To a solution of 4-bromo-2-chloro-pyridine (1.0 g, 5.2 mmol) in DME/water 10:1 (15 mL) was added (2-methoxyphenyl)boronic acid (0.79 g, 5.2 mmol), Pd(PPh3)2Cl2 (240 mg, 0.34 mmol), and K2CO3 (1.8 g, 13.0 mmol). The mixture was heated with reflux for 6 hours. It was diluted with DCM, washed three times with water, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by flash chromatography (silica gel, DCM/MeOH 100:0 to 90:10) to give the title compound A1 (0.6 g, 52%). MS (ES) C12H10ClNO requires: 219. found: 220 (M+H)+.
WORKUP
后处理
- temperatureThe mixture was heated
- temperaturewith reflux for 6 hours
- washwashed three times with water
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
- customThe residue was purified by flash chromatography (silica gel, DCM/MeOH 100:0 to 90:10)