HRID1776066

反应详情

EQUATION

反应方程式

HRID 1776066 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 80 ml of toluene, 20 ml of ethanol, and 40 g of 2M sodium carbonate aqueous solution to 6.50 g of 2,7-dibromocarbazole, 7.32 g of phenyl boronic acid, 0.734 g of tetrakis triphenyl phosphine palladium; reflux the mixture for three hours while heating in nitrogen atmosphere followed by cooling down to room temperature; filter the mixture to remove insoluble matters; distill away the solvent to obtain 4.15 g of pale bark powder of 2,7-diphenyl carbazole; mix 4.01 g of the thus obtained 2,7-diphenyl carbazole, 4.37 g of 4-(8-hydroxyoctyloxy)iodine benzene, 3.45 g of potassium carbonate, 0.5 g of copper powder, and 20 ml of nitrobenzene; reflux the mixture for seven hours while heating in nitrogen atmosphere followed by cooling down to room temperature; filter the mixture to remove insoluble matters; distill away the solvent; next, refine the resultant with silica gel column chromatography using a liquid mixture of ethyl acetate and hexane as an eluting solution to obtain 2.0 g of a pale bark oily matter of 2.7-diphenyl-N-[4-(8-hydroxyoctyloxyphenyl)]carbazole; and then, tosylate, thioacetylate, and hydrolyze the thus obtained 2.7-diphenyl-N-[4-(8-hydroxyoctyloxyphenyl)]carbazole in the same manner as in Synthesis of Carbazole Derivative 2 to obtain 2,7-diphenyl-N-[4-(8-mercaptooctyloxyphenyl)]carbazole (hereinafter referred to as carbazole derivative 5) having a colorless needle-like crystal represented by the chemical structure 11.

WORKUP

后处理

  1. temperaturereflux the mixture for three hours
  2. temperaturewhile heating in nitrogen atmosphere
  3. filtrationfilter the mixture
  4. customto remove insoluble matters
  5. distillationdistill away the solvent