研究目的
Investigating the catalytic effects of a new cobalt(III)/[Mo6O19]2? heterogeneous catalyst on the oxidative coupling of amines to imines under mild conditions.
研究成果
The compound [Co(L)2]2[Mo6O19] (1) serves as an efficient heterogeneous catalyst for the oxidative coupling of amines to imines under mild conditions, with high yield and good recyclability. The kinetic study provided insights into the reaction mechanism, suggesting a synergistic effect between [Co(L)2]+ and [Mo6O19]2?.
研究不足
The study is limited by the need for further optimization of reaction conditions and exploration of the catalyst's applicability to a broader range of substrates.
1：Experimental Design and Method Selection:
The study involved the synthesis of a new compound [Co(L)2]2[Mo6O19] (1) by incorporating 2-acetylpyridine thiosemicarbazone (HL), Co(NO3)2·6H2O, and Na2MoO4·2H2O under solvothermal conditions. The compound was characterized using elemental analysis, IR, UV–Vis, PXRD, XPS, and X-ray single-crystal diffraction.
2：Sample Selection and Data Sources:
The materials used included sodium molybdate dehydrate, cobaltous nitrate hexahydrate, methanol, and chloroform-d. The ligand HL was synthesized as previously described.
3：List of Experimental Equipment and Materials:
Instruments used included a Bruker VERTEX-70 FT-IR spectrophotometer, TU–1900 spectrometer, Rigaku D/Max–2400, ESCALAB 250 XI spectrometer, and Zeiss supra55 SEM.
4：Experimental Procedures and Operational Workflow:
The synthesis was carried out under solvothermal conditions, with the pH adjusted to 2.8. The mixture was heated at 130 °C for 3 days, resulting in red hexagon single crystals.
5：The mixture was heated at 130 °C for 3 days, resulting in red hexagon single crystals. Data Analysis Methods:
5. Data Analysis Methods: The catalytic capability was studied by benzylamine coupling oxidation reaction, with kinetic studies performed to determine the rate law.
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Bruker VERTEX-70 FT-IR spectrophotometer
VERTEX-70
Bruker
Used for collecting IR spectra with an operating range of 400–4000 cm?1.
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Rigaku D/Max–2400
D/Max–2400
Rigaku
Used for taking PXRD data.
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Zeiss supra55
supra55
Zeiss
Used for monitoring the morphology of the compound.
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TU–1900 spectrometer
TU–1900
Used for recording UV–Vis absorption spectrum.
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ESCALAB 250 XI spectrometer
ESCALAB 250 XI
Used for XPS analyses with an Al Kα achromatic X-ray source.
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Varian INOVA-400 MHz type spectrometer
INOVA-400 MHz
Varian
Used for obtaining 1H NMR spectra.
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