HRID888393

反应详情

EQUATION

反应方程式

HRID 888393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of methyl 3-(5-methylpyridin-2-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (0.80 g, 2.27 mmol) in N,N-dimethylformamide (6.8 mL) and water (2.3 mL) were added 2-bromo-3-fluoropyridine (0.44 g, 2.49 mmol), palladium acetate (25.4 mg, 0.11 mmol), 3,3′,3″-phosphinidynetris(benzenesulfonic acid)trisodium salt (0.19 g, 0.34 mmol) and diisopropylamine (0.81 mL, 5.66 mmol). The reaction mixture was heated to 80° C. After 18 h, the mixture was cooled to ambient temperature and the solid was filtered off. Purification by reverse phase HPLC (C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.1% trifluoroacetic acid) gave the title compound. MS 323.0 (M+1).

WORKUP

后处理

  1. temperaturethe mixture was cooled to ambient temperature
  2. filtrationthe solid was filtered off
  3. customPurification by reverse phase HPLC (C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.1% trifluoroacetic acid)