HRID1780558

反应详情

EQUATION

反应方程式

HRID 1780558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

3.35 g (10.00 mmol) of 2-fluoro-6-(4-octyloxyphenyl)pyridine-3-boronic acid in 45 ml of ethanol are refluxed together with 2.85 g (10.00 mmol) of 1-bromo-4-octyloxybenzene and 0.37 g (0.31 mmol) of tetrakis(triphenylphosphine)palladium in 60 ml of benzene and 3.18 g (30.00 mmol) of sodium carbonate in 12 ml of water for 20 hours. After distributing the reaction mixture between water and dichloromethane, the organic phase is washed with sodium chloride solution, dried over sodium sulfate, filtered and concentrated. Purification of the residue by chromatography (silica gel, dichloromethane) and recrystallization from acetonitrile give 2.5 g of 2-fluoro-3,6-di(4-octyloxyphenyl)pyridine. ##STR30##

WORKUP

后处理

  1. washthe organic phase is washed with sodium chloride solution
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customPurification of the residue
  6. customby chromatography (silica gel, dichloromethane) and recrystallization from acetonitrile