反应详情

温度

108 °C

A solution of 68.3 g (381 mmol) of 1-azaphenanthrene and 157 g (470 mmol) of iodopentoxide in acetic acid was stirred under heat at 108° C. for 2 hours. After the reaction liquid had been cooled to room temperature, water was added to the reaction liquid to crystallize the product, and then the crystals were filtered off. Subsequently, the resultant crystal was dissolved in chloroform, washed with an aqueous solution of sodium hydrogen carbonate and an aqueous solution of sodium thiosulfate, dried, and exsiccated by concentration, whereby 53.9 g of 1-azaphenanthrene-5,6-dione were obtained (68% yield).

1. customAfter the reaction liquid
2. temperaturehad been cooled to room temperature
3. customto crystallize the product
4. filtrationthe crystals were filtered off
5. dissolutionSubsequently, the resultant crystal was dissolved in chloroform
6. washwashed with an aqueous solution of sodium hydrogen carbonate
7. dry with materialan aqueous solution of sodium thiosulfate, dried
8. concentrationexsiccated by concentration