ChemicalBook CAS DataBase List Quinocetone

Quinocetone synthesis

4synthesis methods

Product Name:Quinocetone
CAS Number:81810-66-4
Molecular formula:C18H14N2O3
Molecular Weight:306.32

100-52-7

2-ACETYL-3-METHYLQUINOXALINEDIIUM-1,4-DIOLATE

13297-17-1

81810-66-4

In a 250 mL three-neck flask, 64 mL of methanol and 5.05 g (0.0455 mol) of anhydrous CaCl? were added and stirred until completely dissolved. Subsequently, 3.70 g (0.0344 mol) of hydroxyethylamine formate solution was added slowly and dropwise. Next, 20.25 g (0.1908 mol) of benzaldehyde was added, stirred and the temperature of the reaction system was raised to 50 °C. Then, 37.50 g (0.1718 mol) of 2-acetyl-3-methylquinoxaline 1,4-dioxide was added and slowly heated to 60-65 °C and kept at this temperature for 3 hours of reaction. The progress of the reaction was monitored by TLC and the heating was stopped after confirming the completion of the reaction. The reaction mixture was cooled to 25°C and subjected to diafiltration. The resulting solid was washed 3 times with methanol, evacuated and dried under vacuum to give 49.98 g of bright yellow powdery solid product 2-cinnamoyl-3-methylquinoxaline 1,4-dioxide with a melting point of 189-191 °C, purity of 98.7% and yield of 95.0%.

100-52-7 Synthesis

100-52-7
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13297-17-1 Synthesis

13297-17-1
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81810-66-4
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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

480-96-6 Synthesis