Synthesis of Cyclohexanone Ethylene Ketal Catalyzed by Keggin Type Biimidazole Tungstogermanate

doi:10.3724/SP.J.1095.2014.30653

Chinese Journal of Applied Chemistry

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Synthesis of Cyclohexanone Ethylene Ketal Catalyzed by Keggin Type Biimidazole Tungstogermanate

YANG Liu, LU Mingda, ZHANG Lancui^*, ZHANG Bai, SUN Hang, ZHU Zaiming^*

(School of Chemistry and Chemical Engineering,Liaoning Normal University,Dalian 116029,China)

Received:2013-12-23 Revised:2014-03-10 Published:2014-10-09 Online:2014-10-09

Abstract

Abstract: A Keggin-type biimidazole tungstogermanate(H4biim)[H2GeW12O40]·18H2O(1b, H2biim=2,2′-biimidazole), as a catalyst for the synthesis of cyclohexanone ethylene ketal, was designed and synthesized. It was characterized by single crystal X-ray diffraction analysis, infrared spectroscopy(FT-IR), ultraviolet spectroscopy(UV), themogravimetrydifferential thermal analysis(TG-DTA) and X-ray powder diffraction(XRD). Factors, such as the molar ratio of cyclohexanone to ethylene glycol, catalyst loading and reaction time, on the yield were investigated. The experimental results show that the product yield reaches 90% under the optimal conditions:n(cyclohexanone)∶n(1,2-ethanediol)=1∶1.4, n(1b, based on W)∶n(cyclohexanone)=1∶260, reaction time is 2 h. The catalyst can be reused and has good stability in the catalytic reaction.

Key words: Keggin-type Structure, tungstogermanate, biimidazole, carbonyl-protecting reaction, catalysis

CLC Number:

O614.6

YANG Liu, LU Mingda, ZHANG Lancui*, ZHANG Bai, SUN Hang, ZHU Zaiming*. Synthesis of Cyclohexanone Ethylene Ketal Catalyzed by Keggin Type Biimidazole Tungstogermanate[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2014.30653.

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Synthesis of Cyclohexanone Ethylene Ketal Catalyzed by Keggin Type Biimidazole Tungstogermanate

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