反应详情

温度

100 °C

To a 1 L one-necked flask was added a mixture of 30 g (0.13 mol, 68%) 5-nitro-1,10-phenanthroline, 51 g (0.61 mol) potassium oxalate, 12.5% NaOH(aq) 150 ml and 450 ml water. The mixture was then heated to reflux (100° C.) and stirred for 2 hours. After completion of the reaction, the reaction mixture was cooled to room temperature. The reaction mixture was added with 1 L ethyl acetate, stirred for 30 minutes, and filtered to collect the filtrate. The residual solids were added into 300 ml ethyl acetate, stirred for 30 minutes and filtered to collect the filtrate. The combined filtrates were extracted to separate the organic layer, dehydrated by MgSO4, concentrated, and recrystallized from 200 ml methanol, so as to obtain light yellow solids cyclopenta[2,1-b;3,4-b′]dipyridin-5-one 13.3 g (0.07 mol, yield 54%).

1. additionTo a 1 L one-necked flask was added
2. temperatureThe mixture was then heated
3. customAfter completion of the reaction
4. temperaturethe reaction mixture was cooled to room temperature
5. stirringstirred for 30 minutes
6. filtrationfiltered
7. customto collect the filtrate
8. additionThe residual solids were added into 300 ml ethyl acetate
9. stirringstirred for 30 minutes
10. filtrationfiltered
11. customto collect the filtrate
12. extractionThe combined filtrates were extracted
13. customto separate the organic layer
14. concentrationconcentrated
15. customrecrystallized from 200 ml methanol