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Eca 500 2 nmr spectrometer

Manufactured by JEOL
Sourced in Japan, United States

The ECA-500 II NMR spectrometer is a laboratory instrument manufactured by JEOL. It is designed to perform nuclear magnetic resonance (NMR) analysis. The core function of the ECA-500 II is to detect and measure the magnetic properties of atomic nuclei within a sample, providing information about the molecular structure and composition of the material under examination.

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7 protocols using eca 500 2 nmr spectrometer

1

Melting Point and NMR Analysis

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Using an electro-thermal melting point apparatus called the Stuart-SMP30 in open glass capillaries, the uncorrected melting points (°C) were ascertained. Nuclear magnetic resonance (NMR) spectra for 1H and 13C were obtained on a JEOL ECA-500 II NMR spectrometer at 600 MHz and 150 MHz, respectively. The chemical shifts represented in ppm downfield from the internal standard, tetramethylsilane, and the coupling constants (J) are given in Hz. Deuteriodimethyl sulfoxide was used as the solvent (DMSO-d6). The reactions were seen and the purity of the finished products was evaluated using thin-layer chromatography, utilizing silica-gel-precoated aluminum sheets (60 F254, Merck) and visualization with ultraviolet light (UV) at 365 and 254 nm.
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2

Comprehensive Analytical Characterization

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A JEOL ECA-500 II NMR spectrometer was used to record NMR spectra at 500 MHz for 1H and 125 MHz for 13C. DMSO-d6 or CDCl3 were used to dissolve NMR samples. Chemical shifts δ were standardized to the solvent resonances. A Thermo Scientific ISQ Quantum Access MAX Triple Quadrupole system, Xcalibur 2.1 software, and USA Mass Spectrometer were used. Jasco′s FT/IR-6100 spectrophotometer was used to record IR spectra on KBr discs. The “Galen Kamp-type” melting point apparatus was used. Polarimeter models from Rudolph Research Analytical, USA, were used to detect optical rotation. Material for column chromatography: silica gel (Merck, 70–230 mesh), Sephadex LH-20 (Sigma–Aldrich Chemical Co. St. Louis, MO, USA), ODS (RPC18, Merck, Germany), silica gel F254 (Merck, 70–230 mesh). Camag UV lamps at 254 and 366 nm were used to observe the results. For spot detection, AlCl3 or 10% sulfuric acid spray reagents were used independently.
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3

NMR and ESI-MS Spectroscopic Analysis

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A JEOL ECA500-II-NMR spectrometer (Akishima, Japan) recorded NMR spectra at 500 MHz for 1H and 125 MHz for 13C. DMSO-d6 was utilized to dissolve the NMR sample. The chemical shifts were normalized using solvent resonances. Thermo Scientific's ISQ Quantum Access MAX Triple Quadrupole system (Waltham, MA), Xcalibur 2.1 software, and USA Mass Spectrometer were used for the ESI-MS.
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4

Chromatographic Purification and Spectroscopic Analysis

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The utilized media, such as Mueller–Hinton agar (MHA) and Mueller–Hinton broth (MHB), as well as chemicals, were purchased from Oxoid, Hampshire, UK, and Merck, Kenilworth, New Jersey, USA. For column chromatography (CC), we employed Silica gel F254 (Merck, 70–230 mesh) and Sephadex LH-20 (Sigma Aldrich Chemical Co., St. Louis, MO, USA).
NMR spectra for 1H and 13C were acquired using a JEOL ECA500-II-NMR spectrometer. The NMR sample was dis-solved in DMSO-d6. Solvent resonances were used to normalize the chemical changes. The ESI-MS was performed using the USA Mass Spectrometer, Xcalibur 2.1 software, and ISQ Quantum Access MAX Triple Quadrupole system from Thermo Scientific, MA, USA.
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5

Characterization of Cisplatin Injection

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Mylan Pharmaceuticals Co. obtained cisplatin (50 mg/50 mL) injection. All other chemicals and solvents were purchased from Sigma-Aldrich unless otherwise mentioned. For CC, we employed Silica gel F254 (Merck, 70–230 mesh) and Sephadex LH-20 (Sigma–Aldrich Chemical Co., St. Louis, MO, USA).
A JEOL ECA500-II-NMR spectrometer recorded NMR spectra at 500 MHz for 1H and 125 MHz for 13C. DMSO-d6 was utilized to dissolve the NMR sample. The chemical shifts were normalized using solvent resonances. Thermo Scientific’s ISQ Quantum Access MAX Triple Quadrupole system, Xcalibur 2.1 software, and USA Mass Spectrometer were utilized for the ESI-MS.
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6

NMR and ESI-MS characterization

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NMR spectra were recorded at 500 MHz for 1H and 125 MHz for 13C using a JEOL ECA-500 II NMR spectrometer. To dissolve the NMR sample, DMSO-d6 was utilized. The solvent resonances were used to normalize the chemical shifts. The ESI-MS was conducted using Thermo Scientific ISQ Quantum Access MAX Triple Quadrupole system, Xcalibur 2.1 software, and USA Mass Spectrometer.
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7

Characterization of Organic Compounds via Spectroscopic Methods

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Melting points
(°C) were measured in open glass capillaries using a Stuart-SMP30
electro-thermal melting point apparatus and are uncorrected. Nuclear
magnetic resonance (NMR) spectra were obtained on a JEOL ECA-500 II
NMR spectrometer at 500.16 MHz for 1H and 125.77 MHz for 13C; the chemical shifts are expressed in δ (ppm) downfield
from tetramethylsilane as the internal standard; and the coupling
constants (J) are expressed in Hz. Deuteriodimethyl
sulfoxide (DMSO-d6) and deuterochloroform
(CDCl3) were used as solvents. Elemental analyses (C, H,
N, and S) were in good agreement with the proposed structures within
±0.4% of the theoretical values (Table S1, Supporting Information). Monitoring the reactions and checking
the purity of the final products were carried out by thin layer chromatography
using silica-gel-precoated aluminum sheets (60 F254, Merck)
and visualization with ultraviolet light (UV) at 365 and 254 nm. The
reference drug donepezil hydrochloride (CAS 120011-70-3) was purchased
from Sigma-Aldrich Chemie GmbH, Germany. Compounds 9, 11,20 (link) and 25(21 (link)) were prepared following the previously reported
procedures.
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