反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter the reaction
- temperaturethe reaction solution was cooled to room temperature
- washwashed with water
- extractionA water layer was extracted with chloroform
- dry with materialthe extracted solution and an organic layer were dried by magnesium sulphate
- customAfter drying
- filtrationthe mixture was filtrated by suction
- concentrationto concentrate the filtrate
- dissolutionThe obtained solid was dissolved in toluene
- filtrationthis solution was filtrated by suction through Florisil, celite, and alumina
- customcondensed, and 30 g of an objective matter