HRID1757353

反应详情

EQUATION

反应方程式

HRID 1757353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

12.74 g (50.00 mmol) of 2,5-dibromo-3-fluoropyridine, 12.51 g (50.00 mmol) of 4-octyloxybenzeneboronic acid, 0.58 g (0.50 mmol) of tetrakis(triphenylphosphine)palladium(0) and 10.60 g (100 mmol) of sodium carbonate are heated at 80° C. for 3 hours in 375 ml of toluene, 250 ml of ethanol and 125 ml of water. The mixture is subsequently partitioned between aqueous sodium chloride solution and ether, and the organic phase is washed with aqueous sodium chloride solution, dried over sodium sulfate, evaporated and purified by chromatography (silica gel/hexane : ethyl acetate =9:1), giving 13.31 g of 5-bromo-3-fluoro-2-(4-octyloxyphenyl)pyridine. ##STR15##

WORKUP

后处理

  1. customThe mixture is subsequently partitioned between aqueous sodium chloride solution and ether
  2. washthe organic phase is washed with aqueous sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. custompurified by chromatography (silica gel/hexane : ethyl acetate =9:1)