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600 or 500 mhz spectrometer

Manufactured by Bruker
Sourced in Switzerland

The 600 or 500 MHz spectrometer is a laboratory instrument used for nuclear magnetic resonance (NMR) spectroscopy. It generates a strong magnetic field and radio frequency (RF) pulses to excite and detect the nuclear spins of atoms in a sample, providing information about the molecular structure and dynamics of the sample.

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4 protocols using 600 or 500 mhz spectrometer

1

Synthesis and Characterization of Novel Organic Compounds

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All reagents and solvents for the synthesis were purchased from Sigma-Aldrich (USA) and Aladdin (China). The reaction was monitored by column chromatography (200–300 mesh) on silica gel GF254. Melting points were measured and were uncorrected on a Fisher-Johns melting apparatus. Mass spectrometry (MS) was performed by an Agilent 1100 LC-MS (Agilent, Palo Alto, CA, USA).
The 1H-NMR and 13C-NMR spectra data were recorded on a 600 or 500 MHz spectrometer from Bruker Corporation (Switzerland) with TMS as an internal standard.
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2

NMR and HPLC-MS Analysis of Organic Compounds

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All 1H, 13C, and two-dimensional (1H–1H correlation spectroscopy [COSY], heteronuclear single quantum coherence [HSQC] spectroscopy, and heteronuclear multiple-bond correlation [HMBC] spectroscopy) NMR spectra were acquired on a Bruker 600- or 500-MHz spectrometer equipped with a 5-mm triple-resonance cryoprobe at 298 K. Residual solvent signals were used as references (acetone-d6, δH 2.05/δC 29.8, 206.0, and CDCl3, δH 7.26/δC 77.0). HPLC-MS spectra were obtained on an Agilent 6120 quadrupole mass spectrometer using a positive ESI source. Amounts of 10 µl of the test samples were injected for HPLC-MS analysis (Agilent Zorbax Eclipse plus C18 reverse-phase column, 5 µm, 4.6 by 150 mm, 10% to 90% CH3CN in H2O with 01% formic acid for 30 min, 1 ml·min−1). HRESIMS data were obtained using the Agilent 6520 quadrupole time of flight (Q-TOF) LC-MS instrument equipped with an electrospray ionization (ESI) source.
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3

Synthesis of Fluorescent Benzaldehyde Derivatives

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3,4-Dihydroxybenzaldehyde, 1-bromohexadecane, boron trifluoride diethyletherate (BF3·Et2O), trifluoroacetic acid and 2-(diphenylphosphino)benzaldehyde were purchased from J&K Scientific Ltd. 2,4-Dimethyl-pyrrole was obtained from Nanjing Chemlin Chemical Industry Co. Ltd. Sodium hypochlorite (NaClO) and potassium dioxide (KO2), tert-butyl hydroperoxide (TBHP) were supplied by Sigma Aldrich. Other chemicals or solvents were purchased from Sinopharm Chemical Reagent Co. Ltd, such as hydrogen peroxide (H2O2), ferric chloride hexahydrate (FeCl3·6H2O), ferrous sulfateheptahydrate (FeSO4·7H2O), N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), triethylamine (Et3N), dichloromethane (CH2Cl2), et al. All chemicals and solvents were used directly without further purification unless otherwise noted. All air and moisture sensitive reactions were carried out under an argon atmosphere. Dry CH2Cl2 was obtained by refluxing and distilling over CaH2 under nitrogen. triethylamine was obtained by simple distillation.
Nuclear magnetic resonance (NMR) spectra were obtained from a Bruker 500 or 600 MHz spectrometer with TMS as an internal standard operating for 1H, 13C NMR and 31P NMR. Mass spectra were measured with a Bruker ultraflex MALDI TOF MS spectrometer. HRMS data were obtained on an Agilent 6224.
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4

NMR Spectroscopy Characterization Protocol

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NMR spectral data were recorded at room temperature using a Bruker 500 or 600 MHz spectrometer unless stated otherwise. The NMR data are reported as follows: chemical shifts in ppm from an internal tetramethylsilane standard on the δ scale, multiplicity (br=broad, app=apparent, s=singlet, d=doublet, t=triplet, q=quartet, and m=multiplet), coupling constants (Hz), and integration. Analytical thin layer chromatography (TLC) was performed using EMD Reagents 0.25 mm silica gel 60-F plates. “Flash” chromatography on silica gel was performed using Silicycle silica gel (40–63 μm). All reactions were carried out under an atmosphere of nitrogen in glassware that was evacuated and back-filled with nitrogen three times. Reactions were carried out at room temperature unless otherwise indicated. Unless otherwise noted, all reagents were commercially obtained and, where appropriate, purified prior to use. THF, Et2O, DMF and CH2Cl2 were dried by filtration through alumina according to the procedure of Grubbs and coworkers.[78 ] For final compounds the purity was determined by HPLC (Agilent Technologies series 1200).
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