HRID1780553

反应详情

EQUATION

反应方程式

HRID 1780553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

2.00 g (7.44 mmol) of 2-fluoro-6-octyloxypyridine-3-boronic acid, 1.64 g (5.72 mmol) of 1-bromo-4-octyloxybenzene, 0.26 g (0.22 mmol) of tetrakis(triphenylphosphine)palladium(0) and 11.16 ml (22.32 mmol) of 2-molar sodium carbonate solution are refluxed in 20 ml of benzene and 10 ml of ethanol for 6 hours. After distributing the reaction mixture between water and diethyl ether, the organic phase is washed with water, dried over sodium sulfate, filtered and concentrated. Purification of the residue by chromatography (silica gel, 95:5 hexane/ethyl acetate) and recrystallization from acetonitrile give 1.02 g of 2-fluoro-6-octyloxy3-(4-octyloxyphenyl)pyridine. ##STR23##

WORKUP

后处理

  1. washthe organic phase is washed with water
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customPurification of the residue
  6. customby chromatography (silica gel, 95:5 hexane/ethyl acetate) and recrystallization from acetonitrile