Ergocalciferol was purchased from variable commercial sources (Alfa Aesar J62163, AstaTech 44109, Research Products International C20300, Sigma-Aldrich 95220, VWR 101172-472). ((Z)-2-((3S,5R)-3,5-bis((tert-butyldimethylsilyl)oxy)-2-methylenecyclohexylidene) ethyl) diphenylphosphine oxide was purchased from ChemScene (CS-M0003). All moisture or oxygen-sensitive reactions were carried out under a dry nitrogen atmosphere. Reaction temperatures refer to the containing bath temperatures. Reactions were monitored by thin-layer chromatography (TLC) using Merck 60 UV254 silica gel plates (Sigma-Aldrich). Visualization was performed with UV light, cerium molybdate general stain followed by heating, and other methods as noted. Synthesized compounds were purified by normal phase flash chromatography (SPI Biotage, silica gel 230-400 mesh) except where noted. Compound characterization was performed via Shimadzu 2020 LC-MS (single quadrupole) instrument. NMR spectra were recorded on a Bruker Avance 500MHz instrument with compounds dissolved in the specified deuterated solvent. Optical rotations were recorded using Jasco DIP-370 Digital Polarimeter instrument in LCMS grade chloroform or methanol.
Avance 500 mhz instrument
Manufactured by Bruker
Sourced in Switzerland, United States
The Avance 500 MHz instrument is a nuclear magnetic resonance (NMR) spectrometer designed by Bruker. It operates at a frequency of 500 MHz and is used for the analysis and characterization of chemical compounds and materials.
Automatically generated - may contain errors
Lab products found in correlation
U 3010 spectrophotometer, by Hitachi (2 mentions)
Dip 370 digital polarimeter, by Jasco (1 mentions)
Merck 60 uv254 silica gel plates, by Merck Group (1 mentions)
Cary 300bio spectrometer, by Agilent Technologies (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Agilent 6530 accurate mass q tof lc ms system, by Agilent Technologies (1 mentions)
Rp 18 f254s plates, by Merck Group (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
Zorbax sb c18, by Agilent Technologies (1 mentions)
Agilent 1100 series system, by Agilent Technologies (1 mentions)
Acquity uplc h class system, by Waters Corporation (1 mentions)
Ir 200 spectrophotometer, by Thermo Fisher Scientific (1 mentions)
Nexera x2 uhplc lc 30a system, by Shimadzu (1 mentions)
6520 quadrupole time of flight mass spectrometer, by Agilent Technologies (1 mentions)
J 810 circular dichroism spectrometer, by Jasco (1 mentions)
Dsc q1000, by TA Instruments (1 mentions)
Uv 1601 uv vis spectrophotometer, by Shimadzu (1 mentions)
Autoflex 3 smart beam instrument, by Bruker (1 mentions)
11 protocols using avance 500 mhz instrument
1
Synthesis of Vitamin D2 Derivatives
2
Monitoring Reactions of AAO and HMF
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Reactions between AAO and HMF, either in the absence or presence of catalase, were monitored by NMR spectroscopy. Reactions were performed in 5 mm NMR tubes in 50 mM sodium phosphate, pH 6.0, with 10% deuterated water (D2O) at 298 K. The course of the reactions was monitored by acquiring 1H-NMR spectra at different reaction times until the complete conversion was achieved. NMR spectra were recorded by introducing the tube at the different reaction times in a Bruker (Billenica, MA, USA) Avance 500 MHz instrument with the probe (triple resonance TXI) at 288 K to shift the 1H-NMR water signal for avoiding overlapping with the signal of the hydroxymethyl group of HMF. The spectra were referenced with water signal at 4.69 ppm. Spectra of the different furfurals were also acquired at 288 K. The amount of each compound was calculated by integrating characteristic signals at: 4.5, 6.4, and 9.2 ppm for HMF; 5.9, 7.4, and 9.5 ppm for DFF, 6.3 and 9.4 ppm for FFCA, and 6.8 ppm for FDCA (Additional file 1 : Fig. S3).
3
Preparative Purification and Characterization
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Example 2
Medium pressure liquid chromatography was performed using an Isolera One system equipped with a dual wave-length UV detector from Biotage and Biotage SNAP Ultra columns. For purification via preparative TLC, silica gel plates (EMD, 1 mm, 20×20 cm) were used, which contained a fluorescence indicator F254. Column chromatography was carried out using silica gel 60, EMD Millipore. All solvents were purchased from EMD Millipore Corporation and used as obtained. Deionized water was purified by a Millipore Milli-Q filtering system equipped with one carbon and two ion-exchange stages. All mass spectral measurements were performed by an Agilent LC-TOF high resolution TOF analyzer at the University of California-Riverside. All NMR spectra were recorded on a Bruker Avance 500 MHz instrument. Residual solvent signals were used as a reference. All UV measurements were performed on a Cary 300 Bio spectrometer from Varian.
4
Anhydrous THF Drying and Characterization
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Anhydrous tetrahydrofuran was dried using standard experimental procedures. Chemical reagents and other solvents were purchased from Energy Chemical. Melting points of compounds were obtained using an SGW X-4 micromelting point instrument (Uncorrected). NMR spectra were recorded on a Bruker AVANCE-500 MHz instrument in CDCl3. The chemical shifts are given in ppm, and J-values are reported in Hz. High-resolution mass spectra (AB Sciex X500R QTOF) of the intermediates and the final compounds were obtained equipped with an ESI source.
5
Comprehensive NMR and Mass Spectrometric Analysis
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The 1H and 13C, DEPT, HSQC, HMBC, ROESY, and COSY NMR spectra were recorded on a Avance 500 MHz instrument (Bruker, Switzerland). The high-resolution electrospray ionization mass spectra (HR-ESI-MS) were obtained from an Agilent 6530 Accurate-Mass Q-TOF LC/MS system (Agilent Technologies Co., Ltd., Waldbronn, Germany). Semi-preparative HPLC was performed on a Agilent 1100 series system,)using an ODS column (Zorbax SB-C18, 9.4 × 250 mm, 5 µm, Agilent Technologies Inc., Santa Clara, CA, USA). Column chromatography was performed on silica gel (200–300 mesh and 300–400 mesh, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China), SephadexTM LH-20 (GE Healthcare Bio-Sciences AB, Uppsala, Sweden), and octadecyl silica (ODS, 50 μm, YMC Co., Ltd., Tokyo, Japan). Thin-layer chromatography was performed on a precoated GF254 plate (Qingdao Haiyang Chemical Co., Ltd., Qingdao, China), RP-18 F254S plates (Merck, Kenilworth, NJ, USA) and compounds were visualized by spraying with aqueous 10% H2SO4 and then heating for 3–5 min.
6
Spectroscopic Pectin Analysis
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Polymer-bound galacturonic acid contents were analyzed spectrophotometrically using the Blumenkrantz procedure [30] (link). To calculate the degree of esterification of IDF and SDF pectins, quantitative 1 H-NMR spectroscopy was performed [31] (link). A suspension of 20 mg sample in 1.5 mL of 2 M NaOH (in D 2 O) was ultrasonicated for 2 h. Trimethylsilylpropanoic acid-d 4 (0.5 mg•mL -1 ) was added as internal standard. A standard 1 H-NMR pulse program (zg30) was used on a Bruker Avance 500 MHz instrument (Ettlingen, Germany), 32 scans were acquired with 65,536 data points and an acquisition time of 3.28 s, and a relaxation delay of 35 s were applied. The degree of methylation and acetylation was calculated related to uronic acid contents.
7
NMR and Mass Spectrometry Analysis
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On the AVANCE 500 MHz instrument (Bruker, Billerica, MA, USA), 1H and 13C/DEPT-NMR, two-dimensional homonuclear (i.e., COSY), and heteronuclear (i.e., HMQC and HMBC) analyses were carried out. Mass spectrometry was performed on a Waters ACQUITY H-Class UPLC system tandem a Waters Xevo TQ-S triple quadrupole time-of-flight mass spectrometer (Waters Corp., Milford, MA, USA).
8
Acetylation of Wood Powders and Xylans
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Acetylation reaction was performed in 1-allyl-3-methylimidazolium chloride ([amim]Cl, 950 mg), on the extractive-free wood powders (50 mg) and birch xylans with acetyl chloride, as reported by Salanti et al. [16] . The procedure was slightly modified and at the end of the reaction, 200 μL of iodomethane were added and left to react for 15 minutes extra in order to convert the carboxylic acids into methyl esters. The acetylated wood samples were solubilized in THF (1 mg mL -1 ) for GPC analysis and in d 6 -DMSO for NMR analyses (50 mg mL -1 ). Further dilutions with the Cr(acac) 3 /CDCl 3 solution were necessary to achieve the complete solubility of the samples (required optimum dilution: 2000 μL). 31 P NMR spectra were recorded on 800 μL solutions on a Bruker Avance 500 MHz instrument [15] . The 31 P NMR data reported are the average of three experiments. The maximum standard deviation was ±0.02 mmol g -1 (P=0.05, n=3).
9
Comprehensive Analytical Techniques for Compound Characterization
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The UV spectrum and data of absorbance were determined by using a HITACHI U-3010 spectrophotometer (Hitachi Ltd., Tokyo, Japan). The IR spectrum was obtained by using an IR200 spectrophotometer (Thermo Electron Corporation, Waltham, MA). The Circular dichroism spectra were obtained using J-810 Circular Dichroism spectrometer (JASCO Corporation, Japan). Optical rotations were measured with Autopol I automatic polarmeter (Rudolph Research Analytical, Hackettstown, NJ). The NMR spectra were recorded using an AVANCE 500 MHz instrument (Bruker Corporation, Switzerland). All compounds were dissolved in DMSO-d 6 or CDCl 3. Relative molecular mass were recorded by using a 6520 quadrupole-time-of-flight mass spectrometer (Agilent, Palo Alto, CA). Purity was detected on a Nexera X2 UHPLC LC-30A system (Shimadzu, Kyoto, Japan), using a Kromasil C18 column (150 mm × 4.6 mm, 5 μm, Dalian Johnsson Separation Science and Technology Corporation). The oven temperature was maintained at 40 °C. Water containing 0.1% formic acid served as solvent system A, and methanol served as solvent system B. The flow rate was 1.0 mL/min, and injection volume was 5 μL. 96-well microplate reader (HBS-1096A) was purchased from Nanjing Detie Experimental Equipment Co., Ltd. (Nanjing, China).
10
Characterization of Organic Compounds
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Reactions were protected from atmospheric moisture by CaCl 2 drying tubes. Anhydrous Na 2 SO 4 was used for drying organic ex tracts, and all volatiles were removed under reduced pressure. Decomposition points were determined using the TA Instrument DSC Q1000 with samples hermetically sealed in aluminium pans under an argon atmosphere, using heating rates of 5 °C/min. UV/vis spectra were obtained using a Shimadzu UV-1601 UV/vis spectrophotometer and inflections are identified by the abbreviation "inf". IR spectra were recorded on a Shimadzu FTIR-NIR Prestige-21 spectrometer with a Pike Miracle Ge ATR accessory. NMR spectra were recorded on a Bruker Avance 500 MHz instrument. Deuterated solvents were used for homonuclear lock and internal calibration. MALDI-TOF mass spectra were recorded on a Bruker Autoflex III Smartbeam instrument. Elemental analysis was performed on a Perkin Elmer 2400 Series Elemental Analyzer by Stephen Boyer of London Metropolitan University.
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