HRID2072608

反应详情

EQUATION

反应方程式

HRID 2072608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This 3-bromo-4-(2'-methylbutyl)benzoic acid chloride (11.5 g, 0.04 mol) was dropwise added to a mixture of 4-hydroxy-4'-octyloxybiphenyl with anhydrous pyridine under ice cooling, followed by agitating the resulting mixture at 50°-60° C. for 2 hours, adding toluene (100 ml), sufficiently agitating the mixture, washing it with 6N-HCl, then with 2N-NaOH aqueous solution and further with water, further drying over anhydrous MgSO4, distilling off toluene and recrystallizing the residue from a mixture of ethanol (100 ml) with ethyl acetate (60 ml) to obtain 3-bromo-4-(2'-methylbutyl)benzoic acid 4'-octyloxy-4-biphenylyl ester (12.2 g), which exhibited liquid crystalline properties and had the following phase transistion points: ##STR45##

WORKUP

后处理

  1. stirringsufficiently agitating the mixture
  2. washwashing it with 6N-HCl
  3. dry with materialwith 2N-NaOH aqueous solution and further with water, further drying over anhydrous MgSO4
  4. distillationdistilling off toluene
  5. customrecrystallizing the residue
  6. additionfrom a mixture of ethanol (100 ml) with ethyl acetate (60 ml)