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Eca 500 nmr spectrometer

Manufactured by JEOL
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The JEOL ECA 500 NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It provides a magnetic field strength of 500 MHz and is capable of conducting various NMR experiments to analyze the structure and properties of chemical compounds.

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Lab products found in correlation

Combiflash ez prep system, by Teledyne (3 mentions) Siliasep silica flash cartridges, by Teledyne (3 mentions) Ltq orbitrap xl, by Waters Corporation (2 mentions) Sunfire prep c18, by Waters Corporation (1 mentions) μbondapak c18, by Waters Corporation (1 mentions) Xbridge prep c18, by Waters Corporation (1 mentions) Mci gel chp 20p, by Mitsubishi (1 mentions) Thermo qexactive plus mass spectrometer, by Thermo Fisher Scientific (1 mentions) Hplc system, by Agilent Technologies (1 mentions) Galaxie chromatography workstation software, by Agilent Technologies (1 mentions) Isco combiflash rf, by Teledyne (1 mentions) Gemini nx c18, by Phenomenex (1 mentions) Ltq orbitrap xl mass spectrometer, by Thermo Fisher Scientific (1 mentions) Uplc synapt g2 hdms, by Waters Corporation (1 mentions) Cd3od, by Eurisotop (1 mentions) Microtof focus mass spectrometer, by Bruker (1 mentions) 700 mhz nmr spectrometer, by Agilent Technologies (1 mentions) Chloroform, by Merck Group (1 mentions) Triton x 100, by Merck Group (1 mentions) Deuterated chloroform, by Merck Group (1 mentions)

Close spelling variants of this product

ECA-500 spectrometer (46 citations) ECA-500 (45 citations) NMR spectrometer (23 citations) ECA 500 MHz NMR spectrometer (8 citations) ECA-500 II NMR spectrometer (7 citations) ECA-500 FT-NMR spectrometer (4 citations) JNM-ECA 500 series NMR JEOL spectrometer (2 citations)

12 protocols using eca 500 nmr spectrometer

1

Microwave-Assisted Compound Purification and Characterization

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Microwave reactions were performed in a CEM Discover microwave reactor. Flash chromatography relied on the Teledyne Isco CombiFlash® EZ Prep system with Silicycle SiliaSep silica flash cartridges (FLH-R10030B-ISO25). Size-exclusion chromatography was performed on a gravity column packed with Sephadex® LH-20. NMR spectra were collected using a JEOL ECA 500 NMR spectrometer (1H, 1H–1H COSY) at the NMR facility at the University of North Carolina at Greensboro (UNCG) and Agilent 700 MHz NMR spectrometer (13C, 13C–1H HSQC, 13C–1H HMBC) at the Joint School of Nanoscience and Nanoengineering at Greensboro (JSNN). The chemical shifts are reported in parts per million (ppm) and were referenced to the residual solvent peaks. ESI mass spectra were obtained using a Thermo Fisher LTQ Orbitrap XL coupled to a Water's Acquity Ultra Performance Liquid Chromatography (UPLC) stack using a BEH C18 column at UNCG's Triad Mass Spectrometry facility. HPLC analyses were carried out on an Agilent/Hewlett Packard 1100 series instrument (ChemStation Rev. A. 10.02 software) using a Hypersil GOLD C18 column (Thermo 25005-254630, guard 25003-014001) with an A–B gradient (40 min run; 98% → 5% A; A = 0.1% formic acid in water, B = 0.1% formic acid in acetonitrile (MeCN)). Reported retention times are accurate to within ±0.1 min.
Roque JA I.I.I., Barrett P.C., Cole H.D., Lifshits L.M., Shi G., Monro S., von Dohlen D., Kim S., Russo N., Deep G., Cameron C.G., Alberto M.E, & McFarland S.A. (2020). Breaking the barrier: an osmium photosensitizer with unprecedented hypoxic phototoxicity for real world photodynamic therapy †Electronic supplementary information (ESI) available: Supplemental methodology, synthetic characterization (1D and 2D NMR, HPLC, HRMS), spectroscopic characterization (emission, TA), computational predictions (ground and excited states), (photo)biological evaluations, and the various acronyms used in-text. See DOI: 10.1039/d0sc03008b. Chemical Science, 11(36), 9784-9806.
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2

Characterization of Organic Compounds

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The solvents and reagents used in the reactions were commercially sourced and not purified further. A Stuart melting point device was used to measure melting points that was uncorrected. NMR spectra were attained using a JEOL ECA 500 NMR Spectrometer (500 MHz 1H and 126 MHz 13 C NMR), while elemental analysis (% C, H, and N) was accomplished using a PerkinElmer 2400 CHNS analyser. Reaction progress and product mixtures were regularly monitored through thin layer chromatography (TLC) using Aluminium sheets pre-coated with silica gel 60 F254 purchased from Merk.
ElNaggar M.H., Elgazar A.A., Gamal G., Hamed S.M., Elsayed Z.M., El-Ashrey M.K., Abood A., El Hassab M.A., Soliman A.M., El-Domany R.A., Badria F.A., Supuran C.T, & Eldehna W.M. (2023). Identification of sulphonamide-tethered N-((triazol-4-yl)methyl)isatin derivatives as inhibitors of SARS-CoV-2 main protease. Journal of Enzyme Inhibition and Medicinal Chemistry, 38(1), 2234665.
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3

Chromatographic Purification and NMR Characterization

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The NMR spectra were measured with a JEOL ECA 500 NMR spectrometer. Preparative HPLC was performed using a SIMADZU LC-20AT pump, JASCO 830-RI detector, Sugai U-620 column heater, and column of COSMOSIL 5C18 AR-II (5 μm, ϕ10.0 × 250 mm, Nacalai Tasque Inc., Kyoto, Japan), SunFire Prep C18, X-Bridge Prep C18 (5 μm, ϕ10.0 × 250 mm, Waters Co., MA, United States) with a flow rate of 2.0 mL/min and column temperature of 40°C. TLC was performed on pre-coated silica gel 60 F254 (Merck Ltd., Frankfurter, Germany) and detection was achieved by spraying with 10% H2SO4 followed by heating. Column chromatography was carried out on MCI gel CHP-20P (Mitsubishi Chemical Co., Tokyo, Japan), Sephadex LH-20 (GE Healthcare Bioscience Co., Uppsala, Sweden), μ-Bonda Pak C18 (Waters Co., MA, United States), and silica gel 60 (230-400 mesh, Merck Ltd., Frankfurter, Germany).
Pan C., Fujiwara Y., Horlad H., Shiraishi D., Iriki T., Tsuboki J., Ikeda T, & Komohara Y. (2020). Flavonoid Compounds Contained in Epimedii Herba Inhibit Tumor Progression by Suppressing STAT3 Activation in the Tumor Microenvironment. Frontiers in Pharmacology, 11, 262.
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4

NMR and HRMS Analysis of Compounds

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NMR experiments were conducted in DMSO-d6 on a JEOL ECA-500 NMR spectrometer operating at 500 MHz for 1H and 125 MHz for 13C (JEOL USA, Inc., Peabody, MA, USA) (Fig. 8S, Supporting Information). HRESIMS data were obtained using a Thermo QExactive Plus mass spectrometer (ThermoFisher Scientific) paired with an electrospray ionization source.
Graf T.N., Kao D., Rivera-Chávez J., Gallagher J.M., Raja H.A, & Oberlies N.H. (2020). Drug Leads from Endophytic Fungi: Lessons Learned via Scaled Production. Planta medica, 86(13-14), 988-996.
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5

Analytical Characterization of Compounds

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NMR data were collected using a JEOL ECA-500 NMR spectrometer operating at 500 MHz for 1H and 125 MHz for 13C (JEOL Ltd., Tokyo, Japan). Residual solvent signals were utilized for referencing. High resolution mass spectra (HRMS) were obtained using a Thermo LTQ Orbitrap XL mass spectrometer equipped with an electrospray ionization source (Thermo Fisher Scientific, San Jose, CA, USA). Phenomenex Gemini-NX C18 analytical (5 μm; 250 × 4.6 mm) and preparative (5 μm; 250 × 21.2 mm) columns (Phenomenex, Torrance, CA, USA) were used on a Varian Prostar HPLC system equipped with Prostar 210 pumps and a Prostar 335 photodiode array detector (PDA), with data collected and analyzed using Galaxie Chromatography Workstation software (version1.9.3.2, Varian Inc.). Flash chromatography was conducted on a Teledyne ISCO CombiFlash Rf using Silica Gold columns and monitored by UV and evaporative light-scattering detectors (both from Teledyne Isco, Lincoln, NE, USA).
Parlet C.P., Kavanaugh J.S., Crosby H.A., Raja H.A., El-Elimat T., Todd D.A., Pearce C.J., Cech N.B., Oberlies N.H, & Horswill A.R. (2019). Apicidin Attenuates MRSA Virulence through Quorum-Sensing Inhibition and Enhanced Host Defense. Cell reports, 27(1), 187-198.e6.
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6

NMR and Mass Spectrometry Analysis of Tenuazonic Acid

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Nuclear magnetic resonance (NMR) spectra were recorded on a 500-MHz ECA500 NMR spectrometer (JEOL Ltd., Tokyo, Japan) at 293 K. The NMR chemical shifts 1H and 13C were referenced to the solvent peaks: δH 3.30 and δC 49.0 for CD3OD (Eurisotop, Saint-Aubin, France). High-resolution electrospray ionization mass spectrometry (HRESIMS) analysis was performed using UPLC-SYNAPT G2 HDMS (Waters, Milford, MA, United States).
Tenuazonic acid (compound 1): 1H and 13C NMR data – see Supplementary Table S1; HRESIMS m/z: [M + H]+; calculated for C10H16NO3 198.1130, result was 198.1127.
Ninomiya A., Urayama S.I., Suo R., Itoi S., Fuji S.I., Moriyama H, & Hagiwara D. (2020). Mycovirus-Induced Tenuazonic Acid Production in a Rice Blast Fungus Magnaporthe oryzae. Frontiers in Microbiology, 11, 1641.
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7

Analytical Techniques for Coordination Complexes

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Microwave reactions were performed in a CEM Discover microwave reactor. NMR spectra were collected using a 300 MHz Bruker BZH 300/52 spectrometer at Acadia University’s Center for Microstructural Analysis (ACMA) and a JEOL ECA 500 NMR Spectrometer at UNCG’s NMR facility. ESI mass spectra were obtained using a Bruker microTOF focus mass spectrometer (Dalhousie University Mass Spectrometry Laboratory). HPLC analyses were carried out on an Agilent/Hewlett Packard 1100 series instrument (ChemStation Rev. A. 10.02 software) using a Hypersil GOLD C18 reversed-phase column (Thermo 25005–254630, guard 25003–014001) with an A–B gradient (40 min run; 2% → 95% B; A=0.1% formic acid in H2O, B=0.1% formic acid in MeCN; Table S4). The free ligand PCIP was run with the same gradient except with 0.1% formic acid in MeOH instead of MeCN. Reported retention times are accurate to within ±0.1 min.
Roque J I.I.I., Havrylyuk D., Barrett P.C., Sainuddin T., McCain J., Colón K., Sparks W.T., Bradner E., Monro S., Heidary D., Cameron C., Glazer E.C, & McFarland S. (2019). Strained, Photoejecting Ru(II) Complexes that are Cytotoxic Under Hypoxic Conditions. Photochemistry and photobiology, 96(2), 327-339.
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8

Moisture-free Hydroboration Reactions with Diverse Substrates

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All hydroboration reactions were carried
out under a moisture- and oxygen-free nitrogen atmosphere. 1,4-Dioxane,
1,2-dichloroethane (DCE), toluene, hexane, and tetrahydrofuran (THF)
were taken from a solvent purification system (PS-400-5, Unilab Mbraun,
Inc.). Glassware was predried in an oven at 100 °C for several
hours and cooled prior to use. tBuOLi,
esters, lactones, and epoxides were obtained commercially from Energy
Chemical, J&K, Acros Organics, Alfa Aesar, or TCI without further
purification. Melting points are uncorrected and recorded on Digital
Melting Point Apparatus WRS-1B. Compounds 1zp, 2zo-1,
and HBdan were synthesized according to ref (24 (link)). Deuterated solvents were
obtained from Cambridge Isotope. 1H NMR, 13C
NMR, and 11B NMR spectra were recorded on a JEOL ECA-500
NMR spectrometer (FT, 500 MHz for 1H; 125 MHz for 13C; 160 MHz for 11B) at room temperature. All chemical
shift values are quoted in ppm referenced to an internal tetramethylsilane
at 0.00 ppm for 1H NMR and relative to residual CHCl3 at 77.16 ppm for 13C unless otherwise noted. The
following abbreviations were used to describe peak splitting patterns
when appropriate: br = broad, s = singlet, d = doublet, t = triplet,
q = quartet, m = multiplet. Coupling constant (J)
was reported in hertz. GC-MS analyses were measured on a Focus GC-ISQ
MS instrument.
Shi Y., Wang Y., Huang Z., Zhang F, & Shao Y. (2022). tBuOLi-Promoted Hydroboration of Esters and Epoxides. ACS Omega, 7(22), 18876-18886.
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9

NMR Spectroscopy of Trichokonins VII and VIII

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NMR spectral analyses were conducted in DMSO-d6 for purified compounds trichokonins VII and VIII on a JEOL ECA-500 NMR spectrometer operating at 500 MHz for 1D 1H NMR experiments (JEOL Ltd.) or an Agilent 700 NMR spectrometer (Agilent Technologies) operating at 175 MHz for 13C NMR. Residual solvent signals of DMSO-d6 (δH = 2.50 and δC = 39.51) were used for referencing spectra and a tetramethylsilane (TMS) internal reference. MestReNova was used to integrate spectral data.
Winter H.L., Flores-Bocanegra L., Cank K.B., Crandall W.J., Rotich F.C., Tillman M.N., Todd D.A., Graf T.N., Raja H.A., Pearce C.J., Oberlies N.H, & Cech N.B. (2023). What was old is new again: Phenotypic screening of a unique fungal library yields pyridoxatin, a promising lead against extensively resistant Acinetobacter baumannii (AB5075). Phytochemistry letters, 55, 88-96.
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10

Analytical Techniques for Compound Characterization

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Microwave reactions were performed in a CEM Discover microwave reactor. Flash chromatography relied on the Teledyne Isco CombiFlash® EZ Prep system with Silicycle SiliaSep silica flash cartridges (FLH-R10030B-ISO25). Size-exclusion chromatography was performed on a gravity column packed with Sephadex® LH-20. NMR spectra were collected using a JEOL ECA 500 NMR spectrometer (1H, 1H-1H COSY) and JEOL 400 NMR spectrometer (1H) at the NMR facility at the University of North Carolina at Greensboro (UNCG) and Agilent 700 MHz NMR spectrometer (1H-1H COSY) at the Joint School of Nanoscience and Nanoengineering at Greensboro (JSNN). The chemical shifts are reported in parts per million (ppm) and were referenced to the residual solvent peaks. ESI mass spectra were obtained using a Thermo Fisher LTQ Orbitrap XL coupled to a Water’s Acquity Ultra Performance Liquid Chromatography (UPLC) stack using a BEH C18 column at UNCG’s Triad Mass Spectrometry facility. HPLC analyses were carried out on an Agilent/Hewlett Packard 1100 series instrument (ChemStation Rev. A. 10.02 software) using a Hypersil GOLD C18 column (Thermo 25005–254630, guard 25003–014001) with an A–B gradient (40 min run; 98% → 5% A; A=0.1% formic acid in water, B=0.1% formic acid in acetonitrile (MeCN); see Table S1). Reported retention times are accurate to within ± 0.1 min.
Cole H.D., Roque JA I.I.I., Lifshits L.M., Hodges R., Barrett P.C., Havrylyuk D., Heidary D., Ramasamy E., Cameron C.G., Glazer E.C, & McFarland S.A. (2021). Fine-feature Modifications to Strained Ruthenium Complexes Radically Alter Their Hypoxic Anticancer Activity. Photochemistry and photobiology, 98(1), 73-84.
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