All reagents used for the experiments were purchased from Sigma-Aldrich (Munich, Germany) and Merck Co. (Darmstadt, Germany) and used without further purification. They had a class of the purity declared by the manufacturer. The melting points of the obtained compounds were determined with a Fisher–Johns apparatus (Fisher Scientific, Schwerte, Germany), without any correction. The purity of the compounds obtained was assessed through thin layer chromatography (TLC) on plates covered with silica gel (aluminum oxide 60 F-254) by Merck. Chloroform-ethanol mixtures in the ratio 10:1 (v/v) were used as the mobile phase. Spots were developed by irradiation with UV light with a wavelength λ = 254 nm. FT-IR spectra were recorded on a Nicolet 6700 spectrometer (Thermo Scientific, USA); in cm−1. 1H and 13C NMR spectra were recorded on the Bruker Avance 300 and 600 apparatus (Bruker BioSpin GmbH, Hamburg, Germany). The compounds were dissolved in dimethyl sulfoxide (DMSO-d6) for analysis. Tetramethylsilane (TMS) was used as an internal standard. Chemical shift values are given in ppm. Then elemental analyses were determined by a Perkin Elmer 2400 series II CHNS/O analyzer (PerkinElmer, Waltham, MA, USA), and the results were within ±0.4% of the theoretical value.
Aluminum oxide 60 f 254
Manufactured by Merck Group
Sourced in United States
Aluminum oxide 60 F-254 is a chromatographic adsorbent used for thin-layer chromatography (TLC) and column chromatography. It is a form of aluminum oxide with a particle size of 60-mesh and the presence of a fluorescent indicator, F-254, which allows for UV detection of separated compounds.
Automatically generated - may contain errors
Lab products found in correlation
Avance 300 and 600, by Bruker (3 mentions)
Fisher johns apparatus, by Thermo Fisher Scientific (2 mentions)
2400 series 2 chns o analyzer, by PerkinElmer (2 mentions)
Perkin elmer 2400 series 2 chns o analyzer, by PerkinElmer (1 mentions)
Nicolet 6700 spectrometer, by Thermo Fisher Scientific (1 mentions)
N butyllithium, by Kanto Chemical (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
4 protocols using aluminum oxide 60 f 254
1
Synthesis and Characterization of Organic Compounds
2
Synthesis and Characterization of Organic Compounds
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All reagents and solvents used in this research were purchased from Sigma-Aldrich (Munich, Germany) and Merck Co. (Darmstadt, Germany) and used without further purification. Thin-layer chromatography (TLC) on plates covered with silica gel (aluminum oxide 60 F-254, Merck Co., Kenilworth, NJ, USA) was used to check the purity of the obtained compounds and to monitor the progress of the reaction. Chloroform–ethanol mixture in the 10:1 (v/v) ratio was used as the mobile phase. The spots were detected by irradiation with UV light at a wavelength of λ = 254 nm. 1H NMR and 13C NMR spectra were recorded on the Bruker Avance 300 and 600 apparatus (Bruker BioSpin GmbH, Rheinstetten, Germany). The melting points of the obtained compounds were measured with a Fisher–Johns apparatus (Fisher Scientific, Schwerte, Germany) and presented without any correction. The elemental analysis was determined by the Perkin Elmer 2400 series II CHNS/O analyzer (Waltham, MA, USA), and the results were within ±0.4% of the theoretical value.
3
Synthesis and Characterization of Organic Compounds
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All reagents and solvents used in this research were purchased from Sigma-Aldrich (Munich, Germany) and Merck Co. (Darmstadt, Germany) and used without further purification. Thin layer chromatography (TLC) on plates covered with silica gel (aluminum oxide 60 F-254, Merck Co.) was used to check the purity of the obtained compounds and to monitor the progress of the reaction. Chloroform-ethanol mixture in the 10:1 (v/v) ratio was used as the mobile phase. The spots were detected by irradiation with UV light at a wavelength of λ = 254 nm. 1H NMR and 13C NMR spectra were recorded on the Bruker Avance 300 and 600 apparatus (Bruker BioSpin GmbH, Germany). The melting points of the obtained compounds were measured with a Fisher-Johns apparatus (Fisher Scientific, Germany), and presented without any correction. The elemental analysis was determined by the Perkin Elmer 2400 series II CHNS/O analyzer (Waltham, MA, USA), and the results were within ± 0.4% of the theoretical value.
4
Synthesis and Characterization of Copper(II) Complexes
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The reactions were monitored by
TLC using Merck “Aluminum oxide 60 F254 neutral,
aluminum sheets” and Merck “Silica gel 60 F254, aluminum sheets”. Column chromatography was carried out
with the use of Al2O3 (Alumina activated 300,
Nacalai Tesque). The reagents used without additional purification
included 2-bromo-3-formylpyridine (96%, Sigma-Aldrich), 5-bromonicotinaldehyde
(97%, Sigma-Aldrich), 6-bromo-3-formylpyridine (95%, Sigma-Aldrich),
3-bromo-2-methylpyridine (97%, Sigma-Aldrich), 3-bromo-5-methylpyridine
(97%, Sigma-Aldrich), 5-bromo-2-methylpyridine (99%, Sigma-Aldrich), n-butyllithium (1.6 M in n-hexane, Kanto
Chemical Co., INC), ethyl formate (FUJIFILM Wako Pure Chemical Corporation),
and PbO2 (FUJIFILM Wako Pure Chemical Corporation). Cu(hfac)2,33 (link) 2,3-bis(hydroxyamino)-2,3-dimethylbutane,34 (link) and 2-methylnicotin aldehyde, 5-methylnicotin
aldehyde, and 6-methylnicotin aldehyde35 were synthesized by standard procedures. C, H, and N elemental analyses
were carried out on a 2400 CHNS/O Series II System (100V) analyzer.
Thermogravimetric and differential thermal analysis (TG-DTA) for polycrystalline
samples [Cu(hfac)2L5-Me ]2, [Cu(hfac)2L5-Br ]2, and [Cu(hfac)2L6-Me ]2 was performed using SII EXSTAR TGA operating
under dry nitrogen with heating from 300 to 500 K at a rate of 5 K/min.
TLC using Merck “Aluminum oxide 60 F254 neutral,
aluminum sheets” and Merck “Silica gel 60 F254, aluminum sheets”. Column chromatography was carried out
with the use of Al2O3 (Alumina activated 300,
Nacalai Tesque). The reagents used without additional purification
included 2-bromo-3-formylpyridine (96%, Sigma-Aldrich), 5-bromonicotinaldehyde
(97%, Sigma-Aldrich), 6-bromo-3-formylpyridine (95%, Sigma-Aldrich),
3-bromo-2-methylpyridine (97%, Sigma-Aldrich), 3-bromo-5-methylpyridine
(97%, Sigma-Aldrich), 5-bromo-2-methylpyridine (99%, Sigma-Aldrich), n-butyllithium (1.6 M in n-hexane, Kanto
Chemical Co., INC), ethyl formate (FUJIFILM Wako Pure Chemical Corporation),
and PbO2 (FUJIFILM Wako Pure Chemical Corporation). Cu(hfac)2,33 (link) 2,3-bis(hydroxyamino)-2,3-dimethylbutane,34 (link) and 2-methylnicotin aldehyde, 5-methylnicotin
aldehyde, and 6-methylnicotin aldehyde35 were synthesized by standard procedures. C, H, and N elemental analyses
were carried out on a 2400 CHNS/O Series II System (100V) analyzer.
Thermogravimetric and differential thermal analysis (TG-DTA) for polycrystalline
samples [Cu(hfac)2L
under dry nitrogen with heating from 300 to 500 K at a rate of 5 K/min.
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