反应详情

温度

120 °C

In a recovery flask were placed 2-tert-butyl-9,10-bis[4-(5-phenyl-1,3,4-oxadiazol-2-yl)phenyl]anthracene-9,10-diol, 6.0 g (36 mmol) of potassium iodide, and 29 g (83 mmol) of sodium phosphinate monohydrate. They are dissolved by the addition of 50 mL of glacial acetic acid. This solution was stirred at 120° C. for 4 hours. Then, 50 mL of a 50% solution of phosphinic acid was added to this solution, and the mixture was stirred at 120° C. for 1 hour. Then, an aqueous solution of sodium hydrogen carbonate was added to this mixture, followed by stirring. After that, the resulting mixture was suction filtered to give a solid. This solid was washed with ethyl acetate. After that, the resulting solid was dissolved in chloroform, and this solution was washed with a saturated aqueous solution of sodium hydrogen carbonate and with saturated brine. Then, magnesium sulfate was added to the organic layer to thy it.

1. customIn a recovery flask were placed
2. stirringthe mixture was stirred at 120° C. for 1 hour
3. stirringby stirring
4. filtrationfiltered
5. customto give a solid
6. washThis solid was washed with ethyl acetate
7. dissolutionAfter that, the resulting solid was dissolved in chloroform
8. washthis solution was washed with a saturated aqueous solution of sodium hydrogen carbonate and with saturated brine
9. additionThen, magnesium sulfate was added to the organic layer to thy it