HRID751746

反应详情

EQUATION

反应方程式

HRID 751746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under an ambient atmosphere of argon gas, cooling a solution prepared by mixing 18.7 g of N-(4-bromophenyl)-N-phenyl-1-naphthylamine, 100 milliliter of dried ethyl ether and 100 milliliter of dried toluene down to a temperature of −78° C., a hexane solution of 1.6M normal butyllithium in an amount 32.8 milliliter was dripped into the cooled solution. The reacted solution was stirred for 1 hour while warming up to a temperature of 0° C. Cooling the reacted solution down to the temperature of −78° C. again, a solution prepared by dissolving 23.5 g of boric acid triisopropyl into dried ether in an amount of 50 milliliter was dripped down to the cooled solution. The resultant solution was further stirred at a room temperature for 5 hours. Adding 100 milliliter of 1 N hydrochloric acid and after stirring the resultant solution for 1 hour, a water layer was removed. After drying an organic layer with a use of magnesium sulfate, the solvent was distillated away under a reduced pressure. Refining a resultant solid by means of a silicagel column chromatography, 10.2 g of 4-(N-1-naphthyl-N-phenylamino)phenylboronic acid was obtained.

WORKUP

后处理

  1. temperatureUnder an ambient atmosphere of argon gas, cooling a solution
  2. customprepared
  3. temperatureCooling the reacted solution down to the temperature of −78° C. again
  4. customa solution prepared
  5. customa water layer was removed
  6. dry with materialAfter drying an organic layer with a use of magnesium sulfate