HRID1780551

反应详情

EQUATION

反应方程式

HRID 1780551 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium octanolate (previously prepared from 13.02 g (100.00 mmol) of 1-octanol and 69 ml (110.00 mmol) of a 1.6-molar n-butyllithium solution in 40 ml of tetrahydrofuran at 0° C.) and 11.51 g (100.00 mmol) of 2,6-difluoropyridine are refluxed in 40 ml of tetrahydrofuran for 7 hours. The mixture is then distributed between sodium chloride solution and ether, the ether phase is washed twice with sodium chloride, dried over sodium sulfate, filtered and freed from solvent. Purification of the residue by chromatography (silica gel, 9:1 hexane/ethyl acetate) gives 13.48 g (59.80 mmol) of 2-fluoro-6-octyloxypyridine. ##STR21##

WORKUP

后处理

  1. washthe ether phase is washed twice with sodium chloride
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. customPurification of the residue by chromatography (silica gel, 9:1 hexane/ethyl acetate)