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ChemicalBook CAS DataBase List Citraconic anhydride
616-02-4

Citraconic anhydride synthesis

13synthesis methods
Citraconic anhydride was prepared by using alkaline earth metal oxides or alkaline earth metal sulfates as catalysts, and reacting for 1.0-10.0h at a mass ratio of itaconic acid and catalyst of 50:1 to 500:1, a mass ratio of itaconic acid and solvent
-

Yield:616-02-4 99.3%

Reaction Conditions:

with calcium in 5,5-dimethyl-1,3-cyclohexadiene at 120; under 750.075 Torr; for 1.5 h;Reagent/catalyst;

Steps:

1 Example 1
0.1 g of calcium, 20 g of itaconic acid and 20 g of xylene were charged to a reaction flask equipped with a thermometer,Stirrer and oil-water separator reactor,Heated to 120 ° C in an oil bath and subjected to a water splitting reaction for 1.5 h at a reduced pressure of 0.1 MPa.The reaction product was distilled off at a vacuum of 500 Pa and a temperature of 100 ° C for recovery.The recovered product was added to the reactor,10 g of itaconic acid and 0.1 g of calcium were heated in an oil bath to 130 ° C.,Decompression in the vacuum degree of vacuum 0.1h reaction 0.5h. The reaction product was distilled under reduced pressure,In the vacuum 500Pa, the temperature of 75 ° C, the color of the effluent slightly pale yellow that is evaporated solvent,Recyclable to continue to use. The product was collected at 100 ° C and the resulting product was a colorless liquid product, citraconic anhydride, yield 99.3%, purity 99.8%.

References:

Shandong Sidier Chemical Technology Co., Ltd.;Chen Pengyu;Zhu Jiazhen;Yin Chuanxiang;Tian Xu;Zhao Wenchao;Zhao Xinyuan;Wang Jincai CN106831670, 2017, A Location in patent:Paragraph 0015; 0016; 0017; 0018; 0019; 0020; 0021

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