HRID1780554

反应详情

EQUATION

反应方程式

HRID 1780554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

24.00 g (66.60 mmol) of 4-bromo-4'-octyloxybiphenyl in 500 ml of hexane and 160 ml of benzene are stirred at room temperature with 49 ml (78.70 mmol) of a 1.6-molar n-butyllithium solution in hexane under argon for 18 hours. The reaction mixture is then slowly added dropwise at 0° C. under argon to a solution of 5.5 ml (60 mmol) of 2,6-difluoropyridine in 200 ml of tetrahydrofuran. After a reaction time of 5 hours at 0° C., the reaction mixture is evaporated to dryness, the residue is taken up in toluene, and solid components are filtered off. The filtrate is washed with water, dried over sodium sulfate, filtered and freed from solvent. Recrystallization from 8:2 hexane/ethyl acetate gives 5.77 g of 2-fluoro-6-[4-(4-octyloxyphenyl)phenyl]pyridine. ##STR24##

WORKUP

后处理

  1. customAfter a reaction time of 5 hours at 0° C., the reaction mixture is evaporated to dryness
  2. filtrationsolid components are filtered off
  3. washThe filtrate is washed with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customRecrystallization from 8:2 hexane/ethyl acetate