HRID1245174

反应详情

EQUATION

反应方程式

HRID 1245174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

To a solution of methyl 3-(3,4,5,6-tetramethoxy-2-methylbenzyl)-2-(trifluoromethanesulfonyl)oxybenzoate (385 mg, 0.7578 mmol) in toluene (8.6 ml) were added tetrakistriphenylphosphine palladium (26 mg, 0.0224 mmol), aqueous solution of sodium carbonate (2M aqueous solution, 0.99 ml), lithium chloride (64 mg, 1.5097 mmol) and ethanolic solution (1.59 ml) of pyridine-4-boronic acid pinacol cyclic ester (233 mg, 1.1365 mmol) and the mixture was heated with stirring at 95° C. for 16 hours. The reaction solution was diluted with ethyl acetate (100 ml), washed with water and dried and the solvent was evaporated therefrom. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to give the title compound (301 mg, 0.6887 mmol, 91%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. washwashed with water
  3. customdried
  4. customthe solvent was evaporated
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)