反应详情

5.1 g (10 mmol) of 2-bromo-9,10-di(2-naphthyl)anthracene, 2.3 g (12 mmol) of 2-phenyl-1H-benzimidazole, 0.19 g (11.0 mmol) of copper iodide, and 3.6 g (2.0 mmol) of 9,10-phenanthroline were dissolved into a 2 M solution of cesium carbonate in dimethylformamide (DMF), and the whole was refluxed under heating for 48 hours in an argon atmosphere. After the completion of the reaction, the resultant was filtered. The filtrate was poured into 1 L of 10-mass % hydrochloric acid, and the whole was extracted with methylene chloride. An organic layer was taken out and dried with magnesium sulfate, and then the solvent was distilled off under reduced pressure. The resultant solid was purified by means of silica gel column chromatography to obtain 2.2 g of a pale yellow solid (35% yield). Mass spectral analysis confirmed that the solid was a target product. The solid had an m/e of 622 with respect to a molecular weight of 622.24.

1. temperaturethe whole was refluxed
2. temperatureunder heating for 48 hours in an argon atmosphere
3. customAfter the completion of the reaction
4. filtrationthe resultant was filtered
5. additionThe filtrate was poured into 1 L of 10-mass % hydrochloric acid
6. extractionthe whole was extracted with methylene chloride
7. dry with materialdried with magnesium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. customThe resultant solid was purified by means of silica gel column chromatography