Bis(hexafluoroacetylacetonato)copper-(II) [abbreviated as Cu(hfac)2] was prepared and purified by previously described procedures [48 ]. Other chemicals were of the highest purity commercially available and were used as received. The progress of reactions was monitored by thin-layer chromatography (TLC) on Silica gel 60 F254 aluminum sheets with hexane or CHCl3 as the eluent. Column chromatography was carried out on silica gel (0.063–0.200 mm). NMR spectra were recorded for 2a ,b solutions in CDCl3 on Bruker Avance-300 (300.13 MHz for 1H, 282.25 MHz for 19F) and Avance-400 (400.13 MHz for 1H, 100.62 MHz for 13C) spectrometers; chemical shifts (δ) of 1H and 13C{1H} are given in ppm, with the solvent signals serving as the internal standard (δH = 7.24 ppm, δC = 76.9 ppm); the internal standard for 19F spectra was C6F6 (δ = −162.9 ppm). Fourier transform infrared (FT-IR) spectra were acquired in KBr pellets on a Bruker Vector-22 spectrometer. UV-vis spectra were registered on an HP Agilent 8453 spectrophotometer (in 10−5–10−4 M solutions in EtOH). Masses of molecular ions were determined by high-resolution mass spectrometry (HRMS) by means of a DFS Thermo Scientific instrument (EI, 70 eV). Melting points were recorded on a Melter-Toledo FP81 Thermosystem apparatus. Elemental analyses were performed using a Euro EA 3000 elemental analyzer.
Vector 22 spectrometer
Manufactured by Bruker
Sourced in Germany, United States
The Vector 22 spectrometer is a high-performance analytical instrument designed for advanced spectroscopic applications. It is capable of providing precise and reliable measurements across a wide range of spectral regions, enabling researchers and scientists to analyze the composition and properties of various materials accurately. The Vector 22 spectrometer is a versatile tool that can be utilized in a variety of scientific and industrial settings to support research, development, and quality control efforts.
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Lab products found in correlation
Inova 500 spectrometer, by Agilent Technologies (6 mentions)
Avance 400 nanobay, by Bruker (6 mentions)
Ecx 500 nmr spectrometer, by JEOL (5 mentions)
Agilent 6550 ifunnel q tof lc ms, by Agilent Technologies (4 mentions)
Avance 400, by Bruker (3 mentions)
Avance 300, by Bruker (3 mentions)
Q exactive, by Thermo Fisher Scientific (3 mentions)
Vario 3 chn analyzer, by Elementar (3 mentions)
Drx 500, by Bruker (3 mentions)
Axs d8 diffractometer, by Bruker (3 mentions)
Quanta 200 microscope, by Thermo Fisher Scientific (3 mentions)
8453 spectrophotometer, by Agilent Technologies (2 mentions)
Q tof micro mass spectrometer, by Waters Corporation (2 mentions)
Dpx 400 mhz, by Bruker (2 mentions)
Optimelt mpa100 melting point apparatus, by Stanford Research Systems (2 mentions)
3flex surface characterization analyzer, by Micromeritics (2 mentions)
Drx 400, by Bruker (2 mentions)
Uv 254 plates, by Vilber (2 mentions)
Pe 2400 chns o elemental analyzer, by PerkinElmer (2 mentions)
Vl 6 lc, by Vilber (2 mentions)
67 protocols using vector 22 spectrometer
1
Synthesis and Characterization of Bis(hexafluoroacetylacetonato)copper-(II)
2
IR Spectroscopy of Artp1 and Artp2
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The IR spectra of Artp1 and Artp2 were obtained using a Bruker Vector 22 spectrometer (Bruker, Rheinstetten, Germany). All samples were mixed with KBr powder, pressed into pellets at room temperature, and then recorded in the range of 4000 to 400 cm−1.
3
Synthesis and Characterization of ATBDC Ligand
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Commercially available reagents were purchased in high purity and used without further purification. 5-(5-amino-1H-tetrazol-1-yl)-1,3-benzenedicarboxylic acid (H2ATBDC) was synthesized according to the literature method52 (Supplementary Fig. 1 ). 1H NMR and 13C NMR spectra were obtained using a Varian INOVA 500 MHz spectrometer at room temperature. FTIR spectra were performed on a Bruker Vector 22 spectrometer at room temperature. Thermal gravimetric analysis (TGA) was performed under a nitrogen atmosphere with a heating rate of 3 °C min−1 using a Shimadzu TGA-50 thermogravimetric analyzer. PXRD patterns were measured by a Rigaku Ultima IV diffractometer operated at 40 kV and 44 mA with a scan rate of 1.0 deg min−1.
4
Structural Elucidation of Natural Products
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Optical rotations were acquired with a Perkin-Elmer 341 polarimeter. The UV spectra were acquired using a Varian Cary Eclipse 300 spectrophotometer, while the IR spectra were recorded on a Bruker Vector 22 spectrometer with KBr pellets. The NMR spectra were recorded on a Bruker Avance 600 NMR spectrometer with TMS as an internal standard. The HRESIMS measurements were obtained with a Q-TOF Micromass spectrometer (Waters, USA). X-ray crystallographic analysis was performed with a Bruker SMART APEX (II)-CCD diffractometer with Cu Kα radiation (λ = 1.54178 Å). The materials for the CC were silica gel (100–200 mesh; Huiyou Silical Gel Development Co. Ltd., Yantai, China), silica gel H (10–40 μm; Yantai), Sephadex LH-20 (40–70 μm; Amersham Pharmacia Biotech AB, Uppsala, Sweden), and YMC-GEL ODS-A (50 μm; YMC, Milford, MA). Semi-preparative HPLC was conducted on an Agilent 1200 instrument using an Eclipse XDB-C18 column (5 μm, 9.4 × 250 mm). Preparative TLC (0.4–0.5 mm) was conducted on glass plates precoated with silica gel GF254 (Yantai).
5
Synthesis of Chromenone Derivative from Myricetrin
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The melting points of the products were determined on an XT-4 binocular microscope (Beijing Tech Instrument Co.). The 1H NMR and 13C NMR (CDCl3 or DMSO as solvents) spectroscopies were performed on a JEOL-ECX 500 NMR spectrometer at room temperature using TMS as an internal standard. The IR spectra were recorded on a Bruker VECTOR 22 spectrometer using KBr disks. High-performance liquid chromatography mass spectrometry was performed on a Thermo Scientific Q Exactive (USA). Unless noted, all solvents and reagents were purchased from Shanghai Titan Scientific Co., Ltd, and were treated with standard methods. Based on the synthesis procedures described in our previous work [14 (link)], intermediates 1 (2-((5,7-dimethoxy-4-oxo-2-(3,4,5-trimethoxyphenyl)-4H-chromen-3-yl)oxy)aceto-hydrazide) were prepared using myricetrin (5,7-dihydroxy-3-(3,4,5-trihydroxy-6-methyltetrahydro-2H-pyran-2-yl)oxy)-2-(3,4,5-trihydroxyphenyl)-4H-chromen-4-one) as the starting material.
6
Spectroscopic Analysis of Organic Compounds
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Melting points were determined by using an XT-4 binocular microscope (Beijing Tech Instrument Co., China) without correction. IR spectra were recorded on a Bruker VECTOR 22 spectrometer. NMR spectra were recorded in a CDCl3 solvent using a JEOL-ECX 500 NMR spectrometer operating at 500 MHz for 1H, and at 125 MHz for 13C by using TMS as internal standard. Elemental analysis was performed on an Elementar Vario-III CHN analyzer. Silica gel (200–300 mesh) and TLC plates (Qingdao Marine Chemistry Co., Qingdao, China) were used for chromatography. All solvents (Yuda Chemistry Co., Guiyang, China) were analytical grade, and used without further purification unless otherwise noted.
7
Synthesis and Characterization of Quinazolin-4(3H)-one Derivatives
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Melting points of synthesized compounds were determined under an XT-4 binocular microscope (Beijing Tech Instrument Co., China) and were not corrected. The IR were recorded from KBr disks using a Bruker VECTOR 22 spectrometer (Bruker, USA). NMR spectra were obtained on a JEOL-ECX500 NMR spectrometer (JEOL, Japan) at room temperature using tetramethylsilane as an internal standard. Reaction was monitored by thin-layer chromatography (TLC) on silica gel GF245 (400 mesh). Mass spectral studies were performed on a quadrupole/electrostatic field orbitrap mass spectrometer (Thermo Scientific, USA). The micro thermophoresis of the compound and TMV CP was determined by a micro thermophoresis instrument (NanoTemper Tchnologies GmbH, Germany); the fluorescence spectroscopy of the compound interacting with TMV CP was determined by FluoroMax-4 fluorescence spectrometer (HORIBA Scientific, France). All reagents and reactants were purchased from commercial suppliers and were analytical grade or chemically pure. The synthetic route to penta-1,4-diene-3-one oxime ether derivatives containing a quinazolin-4(3H)-one scaffold was shown in Scheme 1 . Intermediates 2 and 7 were prepared according to the reported methods [16 , 31 (link)].![]()
Synthetic route to title compounds
8
Characterization of N-Vinylcarbazole-Based Materials
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N-vinylcarbazole (98%), HSiCl3 (99%), and mesitylene (97%) were purchased from Aladdin Reagent Co., Ltd. (Shanghai, China). Analytical-grade ethanol (99.5%) and hydrofluoric acid (40% aqueous solution) were received from Sinopharm Chemical Reagent Co., Ltd. (SCRC; Shanghai, China). All reagents were used as purchased without further purification. The XRD spectrum was performed on a Bruker D8 Advance instrument (Bruker AXS GmbH, Karlsruhe, Germany) with Cu Kα radiation (λ = 1.5418 Å). TEM images were obtained on a JEM-2100 transmission electron microscope with an acceleration voltage of 200 kV (JEOL, Ltd., Akishima, Tokyo, Japan). The FTIR spectra were measured by a Bruker VECTOR 22 spectrometer (Bruker, Germany) with KBr pellets. The PL and excitation spectra were collected by a Hitachi F-4600 fluorescence spectrophotometer (Hitachi, Ltd., Chiyoda-ku, Japan). The UV-vis absorption spectra were measured by a Shimadzu UV-2700 UV-vis spectrophotometer (Shimadzu Corporation, Kyoto, Japan). The PL lifetime was obtained on a Zolix Omni-λ 300 fluorescence spectrophotometer (Zolix Instruments Co., Ltd., Beijing, China).
9
Characterization of Polymer Precursors
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Hydrogen nuclear magnetic resonance (1H NMR) spectra were determined using a BRUKER-300 spectrometer (Massachusetts, U.S.A.) at 300 MHz in CDCl3 or DMSO-d6.
FT-IR measurements were performed using a Bruker Vector 22 spectrometer (Massachusetts, U.S.A.) at a resolution of 2 cm−1 in the range of 400–4000 cm−1, with the samples in the form of powders (monomers) and thin films (PIs).
High resolution liquid chromatography-mass spectroscopy (HRLC-MS) data were obtained using an Agilent 1290-microTOF-QII (Bruker, Massachusetts, U.S.A.) high resolution mass spectrometer.
Elemental analysis was run on a Vario EL cube CHN recorder analysis instrument (Langenselbold, Germany).
FT-IR measurements were performed using a Bruker Vector 22 spectrometer (Massachusetts, U.S.A.) at a resolution of 2 cm−1 in the range of 400–4000 cm−1, with the samples in the form of powders (monomers) and thin films (PIs).
High resolution liquid chromatography-mass spectroscopy (HRLC-MS) data were obtained using an Agilent 1290-microTOF-QII (Bruker, Massachusetts, U.S.A.) high resolution mass spectrometer.
Elemental analysis was run on a Vario EL cube CHN recorder analysis instrument (Langenselbold, Germany).
10
Material Characterization by Advanced Microscopy
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The morphology of the materials was examined by a FEG250 field-emission scanning electron microscopy (SEM) from Quanta, America. Transmission electron microscopy (TEM) was carried out using a JEM-2100F microscope from JEOL Ltd., Japan. The specific surface area was studied by the Brunauer-Emmett-Teller (BET) method, and the pore size distribution was obtained from the nitrogen adsorption-desorption isotherms using a NOVA 2000e analyser from Quantachrome Instruments, America. Fourier-transformed infrared (FT-IR) spectra were recorded using a VECTOR22 spectrometer from Bruker, Germany.
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