HRID345719

反应详情

EQUATION

反应方程式

HRID 345719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Hydroxy-2(4'-propyl-biphenyl-4-yl)pyrimidine (10 g, 0.034 mol) was dissolved in ethanol (100 ml), followed by adding KOH (2.1 g, 0.037 mol), refluxing the mixture, dropwise adding (S)-6-methyloctyl bromide (7.7 g, 0.037 mol) over about 15 minutes, further refluxing the mixture for 5 hours, distilling off ethanol (80 ml), dissolving the residue in toluene (100 ml), transferring the solution into a separating funnel, sufficiently washing it with a 2N-NaOH aqueous solution, washing it with water until the washing water became neutral, drying the resulting organic layer over anhydrous magnesium sulfate, distilling off toluene and recrystallizing the residue from ethanol (200 ml) to obtain (S)-5-(6'-methyloctyloxy)-2(4'-propylbiphenyl-4-yl)pyrimidine (8.9 g). This product was a liquid crystal and exhibited the following phase transition points (also see Table 1): ##STR86##

WORKUP

后处理

  1. temperaturefurther refluxing the mixture for 5 hours
  2. distillationdistilling off ethanol (80 ml)
  3. dissolutiondissolving the residue in toluene (100 ml)
  4. washsufficiently washing it with a 2N-NaOH aqueous solution
  5. washwashing it with water until the washing water
  6. dry with materialdrying the resulting organic layer over anhydrous magnesium sulfate
  7. distillationdistilling off toluene
  8. customrecrystallizing the residue from ethanol (200 ml)