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ChemicalBook CAS DataBase List Quinocetone
81810-66-4

Quinocetone synthesis

4synthesis methods
13297-17-1 Synthesis
2-ACETYL-3-METHYLQUINOXALINEDIIUM-1,4-DIOLATE

13297-17-1
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Yield:81810-66-4 95%

Reaction Conditions:

with 2?hydroxyethylammonium formate;calcium chloride in methanol at 50 - 65; for 3 h;Concentration;

Steps:

2

in 250 mLIn a three-necked flask,After adding 64 mL of methanol and 5.05 g (0.0455 mol) of anhydrous CaCl2, the mixture was dissolved with stirring and then added dropwise3.70 g (0.0344 mol)HydroxyEthylamineFormateSub-liquid,Further, 20.25 g (0.1908 mol) of benzaldehyde was added, the temperature was raised to 50 ° C with stirring, 37.50 g (0.1718 mol)Acetylmethylquine,Slowly heated to 60-65 ° C,The reaction was incubated for 3 hours, TThe LC traces the reaction to the end point and stops the reaction. Cooling down to 25 ° C, suction filtration,Washed 3 times with methanol,Drained,Vacuum drying,To give 49.98 g of a bright yellow powdery solid,M.p. 189-191 ° C,Product purity 98.7%,Yield 95.0%.

References:

CN105566234,2016,A Location in patent:Paragraph 0016; 0017; 0018

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