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ChemicalBook CAS DataBase List 1 10-PHENANTHROLINE-5 6-DIONE 97

1 10-PHENANTHROLINE-5 6-DIONE 97 synthesis

10synthesis methods
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Yield:27318-90-7 85%

Reaction Conditions:

with sulfuric acid;nitric acid;potassium bromide at 5 - 100; for 6 h;

Steps:

1.4 The fourth step reaction
To a three-necked flask were added 1,10-phenanthroline monohydrate (1.0 g, 5.0 mmol) and potassium bromide (1.0 g, 8.4 mmol)The reaction apparatus was placed under ice-cooling,Slowly stirring 10mL concentrated sulfuric acid and 10mL concentrated nitric acid mixture,The reaction temperature was maintained at 5 ° C,Slowly warming to 100 ,Reaction for 6 hours,The mixture is poured into crushed ice,With 5 ~ 10% sodium hydroxide solution adjusted to 8,Extracted with dichloromethane (3 x 40 mL)Dried over anhydrous sodium sulfate,filter,concentrate,Anhydrous ethanol recrystallization,To obtain 0.85 to 0.89 g of a yellow solid,1,10-phenanthroline-5,6-dione (9),Yield: 80.9-85.0%; m.p. 259-261 ° C

References:

Zhejiang University of Technology;Zhang, Wen;Liu, Jiachun;Cheng, Mei CN106565713, 2017, A Location in patent:Paragraph 0046; 0050

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