Abstract
Nano-NiO and bulk NiO were prepared from Ni(AC)2·4H2O by coordination precipitation using aqueous ammonia and by a solid state reaction, respectively. The nickel oxide particles were characterized by X-ray Diffraction (XRD) and scanning electron microscopy (SEM). The results indicate that nano-sized NiO has a crystal phase with a standard face-centered cubic lattice structure, with a mean particle diameter of about 10 nm. The evaluation of the activity of nickel oxide nanoparticles in the catalytic hydrogenation of 7-methoxy-1-naphthylacetonitrile was carried out. The results demonstrate the efficient synthesis of the title compound by a one-pot catalytic hydrogenation and acetylation with NiO. The NiO nanoparticles displayed superior catalytic activity in the synthesis of agomelatine in the one-pot reaction.The total yield of agomelatine is over 81.8% with a purity of 99.2%, as determined by HPLC. The structure of agomelatine was confirmed by IR, MS, and 1H NMR analysis.
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Acknowledgements
The authors are grateful for the support of financial fund (WKDM201509) from Coal Conversion and New Carbon Materials Hubei Key Laboratory, School of Chemistry and Chemical Engineering, Wuhan University of Science and Technology. The authors are also grateful for the support of experimental analysis instrument from New Drugs Innovation Institute, Wuhan University of Science and Technology.
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Funded by the Natural Science Foundation of Hubei Province (2017CFB680), the Hubei University of Science and Technology Nuclear Technology Special Project (2018-19KZ06), the Open Fund of the State Key Laboratory of Refractories and Metallurgy (Wuhan University of Science and Technology) of China (G201703), and the Key Laboratory of Measurement and Control System for Offshore Environment, Fuqing Branch of Fujian Normal University, Fujian Province University (S1-KF1604)
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Yu, Z., Cheng, Z., **e, C. et al. Synthesis of Agomelatine by One-pot Catalytic Hydrogenation and Acetylation with NiO. J. Wuhan Univ. Technol.-Mat. Sci. Edit. 34, 453–458 (2019). https://doi.org/10.1007/s11595-019-2073-3
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DOI: https://doi.org/10.1007/s11595-019-2073-3