反应详情

温度

85 °C

Subsequently, in a stream of argon, 1.5 L of a 10% aqueous solution of sodium hydroxide was added to 51.0 g (244 mmol) of 1-azaphenanthrene-5,6-dione, and heated and stirred at 85° C. for 90 minutes. After the mixture was cooled to room temperature, the precipitate was filtered out. The filtrate was extracted with chloroform and concentrated, and added to the precipitate, whereby a crude material was obtained. The crude material was purified by chromatography on silica gel with toluene/ethyl acetate=10:1 to give 16.8 g of 4-azafluorene-9-one (37.9% yield).

1. temperatureheated
2. temperatureAfter the mixture was cooled to room temperature
3. filtrationthe precipitate was filtered out
4. extractionThe filtrate was extracted with chloroform
5. concentrationconcentrated
6. additionadded to the precipitate, whereby a crude material
7. customwas obtained
8. customThe crude material was purified by chromatography on silica gel with toluene/ethyl acetate=10:1