HRID2072609

反应详情

EQUATION

反应方程式

HRID 2072609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of this 3-bromo-4-(2'-methylbutyl)benzoic acid 4-octyloxy-4'-biphenylyl ester (5.5 g, 0.01 mol), cuprous cyanide (1.1 g, 0.06 mol) and dimethylformamide (20 ml) was heated to 145°-147° C., following by agitating it for 6 hours, adding a mixture of ferric chloride (4 g), hydrochloric acid (1 ml) and water (7 ml), keeping the mixture at 60°-70° C. for 15 minutes, feeding it into ice water, adding toluene, sufficiently agitating the mixture, transferring it into a separating funnel, several times washing the resulting organic layer with water, drying it over anhydrous MgSO4, distilling off toluene and recrystallizing the residue from ethanol (50 ml) to obtain the objective 3-cyano-4-(2'-methylbutyl)benzoic acid 4'-octyloxy-4-biphenylyl ester (1.7 g). The phase transition points of this product were as follows: ##STR46##

WORKUP

后处理

  1. temperaturewas heated to 145°-147° C.
  2. additionadding
  3. customat 60°-70° C.
  4. customfor 15 minutes
  5. stirringsufficiently agitating the mixture
  6. washseveral times washing the resulting organic layer with water
  7. dry with materialdrying it over anhydrous MgSO4
  8. distillationdistilling off toluene
  9. customrecrystallizing the residue from ethanol (50 ml)