Citation:
LUO Zhi-Wei, GU Hui-Zi, ZHOU Li, YAN Xin-Huan. In-situ Liquid-Phase Catalytic Hydrogenation for N-Alkylation[J]. Chinese Journal of Applied Chemistry,
;2009, 26(10): 1169-1173.
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A clean and efficient method has been developed for N-alkylation of amines catalyzed by Ni-Sn/Al2O3 with alcohol as the alkylation agent and solvent as well as hydrogen-donor. For all the reactions,the temperature was 180 ℃,the pressure was 1.5 MPa,and the flow rate was 1.0 mL/min. The structure of the catalyst was confirmed by X-ray diffraction(XRD) and transmission electron microscopy(TEM). The yields of N-alkylation amines were measured by gas chromatography(GC) while their structures were confirmed by gas chromatography-mass spectrometry(GC-MS). The results show that this catalyst has a great conjoint effect for all the reactions in in-situ hydrogenation for N-alkylation,including dehydrogenation of alcohol and hydrogenation of imine intermediates. The total yields of all the N-alkylation products were quite high,and some even greater than 99%. The catalyst had a long life of more than 480 h.
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