HRID35150

反应详情

EQUATION

反应方程式

HRID 35150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To this 2-(m-fluoro-p-hydroxyphenyl)-5-octylpyridine (2 g, 0.007 mol) were added ethanol (20 ml), KOH (0.4 g, 0.007 mol) and optically active 5-methylheptyl bromide (1.4 g, 0.007 mol), followed by heating the mixture under reflux with stirring for 4 hours, cooling, adding water and toluene, transferring the mixture into a separating funnel, washing the resulting organic layer with 2N-NaOH aqueous solution, washing with water, distilling off the solvent under reduced pressure and recrystallizing the residue in a freezer to obtain the objective optically active (S)-2-p-5-methyl-heptyloxy-m-fluorophenyl)-5-octylpyridine (1.8 g).

WORKUP

后处理

  1. temperatureby heating the mixture
  2. temperatureunder reflux
  3. temperaturecooling
  4. washwashing the resulting organic layer with 2N-NaOH aqueous solution
  5. washwashing with water
  6. distillationdistilling off the solvent under reduced pressure
  7. customrecrystallizing the residue in a freezer