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
PROCEDURE
实验过程
Under a stream of nitrogen, 30.2 g (82.0 mmol) of 4,4′-dibromobenzil, 9.31 g (86.1 mmol) of 1,2-phenylenediamine, and 300 mL of chloroform were put into a 500-mL three-neck flask and a reflux thereof was performed at 80° C. for 5 hours. After the reaction, the reaction solution was cooled to room temperature and washed with water. An aqueous layer was extracted with chloroform and dried with magnesium sulfate together with an organic layer. After the drying, the mixture was suctioned and filtrated, and the filtrate was enriched. The obtained solid was dissolved in toluene, and the resulting solution was subjected to suction filtration with florisil, celite, and alumina. The filtrate was enriched, whereby 30.0 g of a white powder solid of 2,3-bis(4-bromophenyl)quinoxaline that was a subject matter was obtained at a yield of 99%.
WORKUP
后处理
- temperaturea reflux
- customAfter the reaction
- washwashed with water
- extractionAn aqueous layer was extracted with chloroform
- dry with materialdried with magnesium sulfate together with an organic layer
- filtrationfiltrated
- dissolutionThe obtained solid was dissolved in toluene
- filtrationthe resulting solution was subjected to suction filtration with florisil, celite, and alumina
- customwas obtained at a yield of 99%