反应详情

温度

80 °C

In a 500 mL three-necked flask were placed 30 g (82 mmol) of 4,4′-dibromobenzil, 9.3 g (86 mmol) of 1,2-phenylenediamine, and 300 mL of chloroform. This solution was refluxed at 80° C. for 5 hours under a stream of nitrogen. After a predetermined time, the solution was cooled to room temperature, and water was added thereto. This aqueous layer was extracted with chloroform, and the extracted solution was combined with the organic layer and then dried with magnesium sulfate. After drying, the mixture was subjected to suction filtration and the filtrate was concentrated. The obtained solid was dissolved in toluene, and this solution was subjected to suction filtration through Florisil (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 540-00135), Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855) and alumina. The filtrate was concentrated, and 30 g of a white powder of 2,3-bis(4-bromophenyl)quinoxaline, which was a target substance, was obtained at a yield of 99%.

1. customIn a 500 mL three-necked flask were placed
2. temperatureAfter a predetermined time, the solution was cooled to room temperature
3. extractionThis aqueous layer was extracted with chloroform
4. dry with materialdried with magnesium sulfate
5. customAfter drying
6. filtrationthe mixture was subjected to suction filtration
7. concentrationthe filtrate was concentrated
8. dissolutionThe obtained solid was dissolved in toluene
9. filtrationthis solution was subjected to suction filtration through Florisil (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 540-00135), Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855) and alumina
10. concentrationThe filtrate was concentrated
11. customwas obtained at a yield of 99%