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ChemicalBook CAS DataBase List 2,3-Dimethoxy-5-methyl-p-benzoquinone

2,3-Dimethoxy-5-methyl-p-benzoquinone synthesis

11synthesis methods
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Yield:605-94-7 99%

Reaction Conditions:

with dipotassium peroxodisulfate;formic acid in methanol;water at 60; for 2.16 h;Reagent/catalyst;Temperature;Solvent;

Steps:

1-5 Example 2
Weigh 3,4,5-trimethoxytoluene (1.82g, 0.01mol) and dissolve it in 5mL methanol, add 0.5mL formic acid, and slowly drop 10mL aqueous solution containing 0.015mol potassium persulfate through a constant pressure dropping funnel. Finish the drop within 10 minutes, react at 60 °C, monitor TLC every half hour, react for 2 hours, stop the reaction, add 10 mL of water to quench the reaction. It was extracted three times with 30 mL of dichloromethane, and the organic layer was washed three times with 15 mL of saturated sodium bicarbonate aqueous solution, and washed with pure water until neutral. Combine the organic phases, dry the organic phases with anhydrous sodium sulfate, and finally filter, spin dry, and recrystallize with n-hexane to obtain red needle-like crystals, namely Coenzyme Q0 (yield 99%).

References:

Yancheng Normal College;Wang Jin;Hu Xiao;Luo Wanyue;Qiu Yongfu;Zhou Rongye;Zhang Nannan;He Yongjing;Zhao Shiyuan;Wang Dingyu;Lu Xin;Li Manyu;Pan Yanhua CN111807945, 2020, A Location in patent:Paragraph 0025-0032

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