The reactions were performed using commercial reagents, and ACS grade solvents used for reactions were purified and dried in accordance with standard procedures. Column chromatography was performed on silica gel 60 (70–230 mesh), and reactions were monitored by TLC on Kieselgel 60 F254. The compounds were detected by examination under UV light and by charring with 5% sulfuric acid in methanol. Solvents were removed under reduced pressure at <40 °C. CH2Cl2 was distilled from CaH2 directly prior to application. Pyridine was dried by refluxing with CaH2 and then distilled and stored over molecular sieves (3 Å). Anhydrous DMF were used without further conditioning. Optical rotations were measured by using a Jasco P-1020 polarimeter. Unless noted otherwise, 1H NMR spectra were recorded in CDCl3 at 300 MHz (Bruker Advance) or at 500 MHz (Bruker ARX-500), 13C NMR spectra and two-dimensional experiments were recorded in CDCl3 at 75 MHz (Bruker Advance) or at 125 MHz (Bruker ARX-500). The 1H NMR chemical shifts are referenced to tetramethylsilane (TMS, δH = 0 ppm) or CDCl3 (δH= 7.26 ppm) for 1H NMR spectra for solutions in CDCl3. The 13C NMR chemical shifts are referenced to the central signal of CDCl3 (δC = 77.00 ppm) for solutions in CDCl3. Accurate mass spectrometry determinations were performed using an Agilent 6230 ESI TOF LCMS mass spectrometer.
Arx 500
Manufactured by Bruker
Sourced in Germany
The ARX-500 is a high-performance nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It is capable of operating at a frequency of 500 MHz, making it suitable for various applications in chemical analysis and structural characterization.
Automatically generated - may contain errors
Lab products found in correlation
Arx 600, by Bruker (2 mentions)
6230 esi tof lc ms mass spectrometer, by Agilent Technologies (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
Arx 400, by Bruker (1 mentions)
Q500 analyzer, by TA Instruments (1 mentions)
Lambda 750 uv vis spectrometer, by PerkinElmer (1 mentions)
C18 column, by Phenomenex (1 mentions)
Lcms it tof, by Shimadzu (1 mentions)
C18 column, by YMC (1 mentions)
Lct premier, by Waters Corporation (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Av 600, by Bruker (1 mentions)
Gct premier spectrometer, by Waters Corporation (1 mentions)
Lct premier xe, by Waters Corporation (1 mentions)
Infinitylab lc msd system, by Agilent Technologies (1 mentions)
Uv 1800pc spectrophotometer, by MAPADA (1 mentions)
8 protocols using arx 500
1
Characterization of Synthetic Compounds
2
Organic Synthesis and Characterization
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All air and water sensitive reactions were performed under a nitrogen atmosphere. Tetrahydrofuran and toluene were dried over Na/benzophenone ketyl and were freshly distilled prior to use. The other materials were of the common commercial level and were used as received. Thin layer chromatography (TLC) was conducted on flexible sheets precoated with SiO2 and the separated products were visualized by UV light. Column chromatography was conducted using SiO2 (300 mesh) from Fisher Scientific. 1H and 13C NMR spectra were recorded on a Bruker ARX-400 (400 MHz) or ARX-500 (500 MHz) spectrometer, using CDCl3. All chemical shifts were reported in parts per million (ppm). The 1H NMR chemical shifts were referenced to TMS (0 ppm), and the 13C NMR chemical shifts were referenced to CDCl3 (77.23 ppm). HR-ESI-MS data were recorded on a Bruker APEX IV mass spectrometer. Thermal gravimetric analysis (TGA) was carried out on a TA Instrument Q500 analyzer. Absorption spectra were recorded on a PerkinElmer Lambda 750 UV-vis spectrometer. Photoluminescence was recorded on a Perkin-Elmer LS 55 spectrofluorometer and a HORIBA JobinYvon Nanolog FL3-2iHR spectrometer.
3
Identification and Characterization of Bioactive Compounds
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1D and 2D- nuclear magnetic resonance spectroscopy (NMR) spectra were recorded on Bruker ARX-500 and ARX-600 spectrometers with tetramethylsilane (TMS) as an internal standard. High-resolution electrospray ionization mass spectroscopy (HR-ESI-MS) was employed on a Shimadzu LCMS-IT-TOF (Kyoto, Japan). 2-Methyl resorcinol, 2-methyl hydroquinone, 5-methyl resorcinol, 1,2,4-benzenetriol, and phosphotungstic acid (H3PW12O40) were purchased from Aladdin Industrial Corporation (Shanghai, China). The melting point was obtained on a micro-melting point apparatus (X-6, Tektronix, USA). An HPLC (1260 system, Agilent, USA) system equipped with a C18 column (250 × 4.6 mm, 5 μm; Phenomenex Synergi, USA) was used, and a semi-preparative RP-HPLC method was conducted with a C18 column (250 × 10 mm, 5 μm; YMC Co., Ltd.). The rat liver was homogenized by a homogenizer (T10, IKA, Germany), and the mitochondria were isolated on a high-speed freezing centrifuge (TGL 20br, Anting, Shanghai, China). Phosphate buffer saline (PBS, pH 7.4), used to isolate the rat liver, was purchased from Haibiao Technology Company (Xiamen, China). A monoamine oxidase assay kit was purchased from Nanjing Jiancheng Bioengineering Institute (Nanjing, China). A Bradford protein quantitation assay kit was purchased from KeyGEN Biotechnology Company (Nanjing, China).
4
Microwave-assisted Synthesis of Novel Compounds
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All reagents and solvents were used as purchased from commercial suppliers or were purified/dried according to Armarego and Chai [28 ]. Purifications by column chromatography on silica gel were performed using Merck Silica Gel 60 (70–230 mesh). 1H and 13C NMR spectra were recorded on Bruker ARX500 instruments using CDCl3 as an internal reference. Chemical shifts (δ values) are given in parts per million (ppm), and the multiplicity of signals is reported as follows: s, singlet; bs, broad singlet; d, doublet; t, triplet; q, quartet; dd, doublet of doublets; m, multiplet. HRMS analyses were performed using a Waters LCT Premier instrument by positive ion mode ElectroSpray Ionization (ESI+). A Monowave 50 appartus from Anton-Paar was used with a thermic control (Pmax: 315 W).
5
Spectroscopic characterization of compounds
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1H and 13C nuclear magnetic resonance spectra were obtained on Bruker ARX500 (500 MHz for 1H and 125 MHz for 13C) or Bruker AV600 (600 MHz for 1H and 150 MHz for 13C) spectrometers (see the electronic supplementary material). Mass spectra were recorded with a Waters GCT Premier spectrometer using electrospray ionization (ES).
6
NMR Characterization of Chemical Compounds
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Nuclear magnetic resonance spectra were recorded using a Bruker ARX500 (500.13 MHz for 1H and 125.77 MHz for 13C) or Bruker ARX 600 (600.13 MHz for 1H, 150.90 MHz for 13C) spectrometer at ambient temperature. 1H and 13C NMR chemical shifts were referenced to solvent resonance of the solvent (DMSO). When necessary, assignments were determined by 1H–13C HSQC (heteronuclear single quantum correlation) and 1H–13C HMBC (heteronuclear multiple bond coherence) spectra. Microanalyses were performed by The School of Chemistry and Molecular Bioscience, University of Queensland, Australia. High-resolution mass spectra were measured using Agilent LCMS 6510 Q-TOF and Waters LCT Premier XE spectrometers using the APCI method with MeCN : H2O (9 : 1) as the solvent.
7
Synthesis and Characterization of Peptide Derivatives
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The peptide derivatives Rh‐GFFYE, Ac‐GFFYE, and Nap‐GFFYE were prepared similarly to our previous study.[19 ] Briefly, they were synthesized by standard Fmoc solid‐phase peptide synthesis (SPPS), which used 2‐chlorotrityl chloride resin and the corresponding N‐Fmoc protected amino acids with side chains suitably protected by a tert‐butyl group or tert‐butyloxycarbonyl group. The resulting crude products were purified by high‐performance liquid chromatography (HPLC, LUMTECH, German) and lyophilization. These compounds were characterized by 1H‐NMR (Bruker ARX 500) and MS. MS was conducted at the Agilent InfinityLab LC/MSD system.
8
Structural Analysis of PEI-based Derivatives
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Fourier transform infrared (FTIR) spectroscopy was used to study the changes in the structures of PEI, PEI-PO and PEI-PO-NONOates using a PE GX Fourier transform infrared spectrometer (PerkinElmer, Boston, MA, USA). The UV-vis absorption peak strength of [N(O-)NvO]-at a wavelength of 250 nm was measured by immersing PEI-PO-NONOates in PBS (0.15 mg mL -1 ) using a UV-1800PC spectrophotometer (MAPADA, Shanghai, China). Subsequently, the chemical structures of PEI, PEI-PO and PEI-PO-NONOates were further determined by nuclear magnetic resonance ( 1 H-NMR and 13 C-NMR) in D 2 O using a 500 MHz NMR spectrometer (Bruker ARX 500, Germany).
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