HRID888702

反应详情

EQUATION

反应方程式

HRID 888702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

30.2 g of 4,4′-dibromobenzil (82.0 mmol), 9.31 g of 1,2-phenylenediamine (86.1 mmol), and 300 mL of chloroform were put into a 500 mL three-necked flask. This reaction solution was refluxed for five hours at 80° C. under a nitrogen gas stream. After the reaction, the reaction solution was cooled to room temperature and washed with water. A water layer was extracted with chloroform, the extracted solution and an organic layer were dried by magnesium sulphate. After drying, the mixture was filtrated by suction to concentrate the filtrate. The obtained solid was dissolved in toluene and this solution was filtrated by suction through Florisil, celite, and alumina. The filtrate was condensed, and 30 g of an objective matter, a white powder solid, 2,3-bis(4-bromophenyl)quinoxaline was obtained at the yield 99%.

WORKUP

后处理

  1. customAfter the reaction
  2. temperaturethe reaction solution was cooled to room temperature
  3. washwashed with water
  4. extractionA water layer was extracted with chloroform
  5. dry with materialthe extracted solution and an organic layer were dried by magnesium sulphate
  6. customAfter drying
  7. filtrationthe mixture was filtrated by suction
  8. concentrationto concentrate the filtrate
  9. dissolutionThe obtained solid was dissolved in toluene
  10. filtrationthis solution was filtrated by suction through Florisil, celite, and alumina
  11. customcondensed, and 30 g of an objective matter