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400 mhz spectrometer

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The 400 MHz spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed to provide precise and reliable analysis of chemical compounds. It operates at a frequency of 400 MHz, which is a common standard in the industry. The core function of this spectrometer is to generate a strong magnetic field and detect the resonant frequencies of nuclei within a sample, enabling the identification and characterization of various chemical structures.

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Lab products found in correlation

Mel temp apparatus, by Merck Group (2 mentions) Type 60 gf254, by Merck Group (2 mentions) 8201 pc ftir spectrophotometer, by Shimadzu (2 mentions) Cary 50 uv vis spectrophotometer, by Agilent Technologies (2 mentions) Jms 600h spectrometer, by JEOL (1 mentions) Smart apex 2 d8 venture diffractometer, by Bruker (1 mentions) 300 mhz spectrometer, by Bruker (1 mentions) 2400 elemental analyzer, by PerkinElmer (1 mentions) Esi qtof mass spectrometer, by Bruker (1 mentions) Isolera one flash purification system, by Biotage (1 mentions) Avance 500 mhz, by JEOL (1 mentions) Ecx 500 spectrometer, by JEOL (1 mentions) Ltq orbitrap xl, by Thermo Fisher Scientific (1 mentions) 500 mhz spectrometer, by Bruker (1 mentions) Specord 40, by Analytik Jena (1 mentions) Agilent 6210 esi tof, by Agilent Technologies (1 mentions) Spectrum two spectrometer, by PerkinElmer (1 mentions) Lcq deca xp max, by Thermo Fisher Scientific (1 mentions) Ultimate 3000 system, by Phenomenex (1 mentions) Dfs mass spectrometer, by Thermo Fisher Scientific (1 mentions)

26 protocols using 400 mhz spectrometer

1

NMR and Mass Spectrometry of Spiroxindole Analogs

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1H-NMR and 13C-NMR spectra of spiroxindole analogs 2a, b were recorded on CDCl3 using a JEOL 400 MHz spectrometer (JEOL Ltd., Tokyo, Japan) at room temperature. Mass spectra were recorded on JMS-600 H JEOL spectrometer (JEOL Ltd., Tokyo, Japan). X-Ray crystallographic analysis was collected by using a Bruker SMART APEX II D8 Venture diffractometer at Karachi University. Note for refractive index (specific rotation) measurement: The samples were prepared in 10 ml, then the concentration was calculated in g/100 ml, and a 100-mm polarimeter tube was used. The instrument used was A.KRÜSS Optronic P8000-PT digital polarimeter.
(E)-3-(3-Fluorophenyl)-1-(1-methyl-1H-pyrrol-2-yl)prop-2-en-1-one 1a and (E)-1-(1-methyl-1H-pyrrol-2-yl)-3-(3-nitrophenyl)prop-2-en-1-one 1b were synthesized according to the literature, and the spectrum is in good agreement with the reported (Yenupuri, et al., 2014 (link)).
Aziz Y.M., Lotfy G., Said M.M., El Ashry E.S., El Tamany E.S., Soliman S.M., Abu-Serie M.M., Teleb M., Yousuf S., Dömling A., Domingo L.R, & Barakat A. (2021). Design, Synthesis, Chemical and Biochemical Insights Into Novel Hybrid Spirooxindole-Based p53-MDM2 Inhibitors With Potential Bcl2 Signaling Attenuation. Frontiers in Chemistry, 9, 735236.
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2

Microwave-Assisted Organic Synthesis

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All reagents and solvents were purchased from commercial suppliers and were used without further purification. 1H-NMR and 13C-NMR spectra were recorded on a JEOL 400 MHz spectrometer (JEOL, Ltd, Tokyo, Japan), and chemical shift (δ) values are expressed in ppm. Mass spectra were recorded on a JEOL JMS-600 H (JEOL, Ltd, Tokyo, Japan). Elemental analyses were carried out on an Elmer 2400 CHNS Elemental Analyzer (PerkinElmer, Inc.940 Winter Street, Waltham, MA, USA). Melting points were measured on a Gallenkamp melting point apparatus (Sigma-Aldrich Chemie GmbH, 82024 Taufkirchen, Germany) in open glass capillaries and are uncorrected. Experiments were performed in a multimode reactor (Synthos 3000, Aton Paar GmbH, 1400 W maximum magnetron, Germany). The vessel was purged with nitrogen gas for 1 min and then placed in the corresponding rotor fixed with a screw; the rotor was then closed with a protective hood. After heating for 6–8 min (600 W at 60 °C), cooling was accomplished by a fan for 5 min.
Almarhoon Z., Dahlous K.A., Abd Alhameed R., Ghabbour H.A, & El-Faham A. (2019). A Simple, Efficient, and Eco-Friendly Method for the Preparation of 3-Substituted-2,3-dihydroquinazolin-4(1H)-one Derivatives. Molecules, 24(22), 4052.
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3

NMR Relaxometry of Gadolinium Complexes

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1H-NMR and 13C-NMR data were obtained using a 300 MHz Bruker spectrometer, Bruker, Covnetry, UK and 29Si NMR were recorded on a JEOL 400MHz spectrometer JEOL, Welwyn Garden City, UK. The longitudinal water proton relaxation rates of the complexes were measured at 59.97 MHz and at 25 °C on a Bruker mq 60 NMR analyser. Gadolinium complexes and GdCl3 were dissolved in ultra-pure water buffered to pH = 7.5 using MOPS 10 mM.
Bruce J.I., O’Connell P.J., Taylor P.G., Smith D.P., Adkin R.C, & Pearson V.K. (2020). Synthesis of Organosilicon Ligands for Europium (III) and Gadolinium (III) as Potential Imaging Agents. Molecules, 25(18), 4253.
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4

Synthesis of Spirooxindole-Phenylsulfone Derivatives

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The 1H-NMR and 13C-NMR spectra of 4a–n were recorded on a JEOL 400-MHz spectrometer (JEOL, Ltd, Tokyo, Japan) at ambient temperature. DMSO-d6 was used as the solvent; the chemical shifts (δ) are given in ppm.
Synthesis of the Spirooxindole-Based Phenylsulfone 4a–n (GP1)A mixture of phenyl vinyl sulfone 1 (0.5 mmol), isatin derivatives 2a–h (0.5 mmol), and amino acids 3a–c (0.5 mmol) in methanol (10 mL) was refluxed in an oil bath for the appropriate time of 8 h. After completion of the reaction, as evident from TLC, the reaction was maintained at room temperature overnight, and the solid crystalline product was filtered off without any further purification.
Barakat A., Mostafa A., Ali M., Al-Majid A.M., Domingo L.R., Kutkat O., Moatasim Y., Zia K., Ul-Haq Z, & Elshaier Y.A. (2022). Design, Synthesis and In Vitro Evaluation of Spirooxindole-Based Phenylsulfonyl Moiety as a Candidate Anti-SAR-CoV-2 and MERS-CoV-2 with the Implementation of Combination Studies. International Journal of Molecular Sciences, 23(19), 11861.
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5

Characterization of Organic Compounds

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All reagents and solvents were purchased from commercial suppliers and used without further purification. The reaction was followed up and checks of the purity were done using TLC on silica gel-protected aluminum sheets (Type 60 GF254, Merck, Darmstadt, Germany). Melting points were recorded on a Mel-Temp Apparatus (Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany) in an open capillary and are uncorrected. Fourier transform infrared spectroscopy (FTIR) was conducted on a Shimadzu 8201 PC FTIR spectrophotometer (Shimadzu, Ltd., Kyoto, Japan). 1H NMR and 13C NMR spectra were recorded on a JEOL 400 MHz spectrometer (JEOL, Ltd., Tokyo, Japan), and chemical shift (δ) values were expressed in ppm. Elemental analyses were performed on a Perkin–Elmer 2400 elemental analyzer (PerkinElmer, Inc., Waltham, MA, USA). High resolution mass spectrometry (HRMS) was performed using a Bruker ESI-QTOF mass spectrometer (Bruker, Billerica, MA, USA) in positive-ion mode.
Shawish I., Barakat A., Aldalbahi A., Alshaer W., Daoud F., Alqudah D.A., Al Zoubi M., Hatmal M.M., Nafie M.S., Haukka M., Sharma A., de la Torre B.G., Albericio F, & El-Faham A. (2022). Acetic Acid Mediated for One-Pot Synthesis of Novel Pyrazolyl s-Triazine Derivatives for the Targeted Therapy of Triple-Negative Breast Tumor Cells (MDA-MB-231) via EGFR/PI3K/AKT/mTOR Signaling Cascades. Pharmaceutics, 14(8), 1558.
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6

Analytical Characterization of Compounds

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All reagents and solvents purchased from commercial suppliers and used without further purification. 1H-NMR and 13C-NMR spectra were recorded on a JEOL 400 MHz spectrometer (JEOL, Ltd., Tokyo, Japan), and chemical shift (δ) values were expressed in ppm. Elemental analyses performed on Perkin–Elmer 2400 elemental analyzer (PerkinElmer, Inc.940 Winter Street, Waltham, MA, USA). Melting points were recorded on a Mel-Temp apparatus Sigma-Aldrich Chemie GmbH, 82024 Taufkirchen, Germany) in an open capillary and are uncorrected. Fourier transform infrared spectroscopy (FTIR) recorded on Shimadzu 8201 PC FTIR spectrophotometer (Shimadzu, Ltd., Kyoto, Japan). The reaction was follow-up and checks of the purity using thin layer liquid chromatograph (TLC) on silica gel-protected aluminum sheets (Type 60 GF254, Merck).
Al Rasheed H.H., Malebari A.M., Dahlous K.A., Fayne D, & El-Faham A. (2020). Synthesis, Anti-proliferative Activity, and Molecular Docking Study of New Series of 1,3-5-Triazine Schiff Base Derivatives. Molecules, 25(18), 4065.
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7

NMR Spectroscopic Analysis Protocol

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1H and 13C NMR spectra were acquired on a Jeol 400 MHz spectrometer (JEOL USA, Inc., Peabody, MA, USA) at 400 and 100 MHz, respectively. Fully decoupled 13C NMR spectra were reported. Chemical shifts were reported in ppm (parts per million) units relative to the internal standard tetramethylsilane (TMS = 0.00 ppm), and the splitting patterns were described as follows: s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), and br was added for broad signals.
Alfei S, & Zuccari G. (2022). One-Step, Low-Cost, Operator-Friendly, and Scalable Procedure to Synthetize Highly Pure N-(4-ethoxyphenyl)-retinamide in Quantitative Yield without Purification Work-Up. Molecules, 27(11), 3632.
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8

Spectroscopic and Elemental Analysis Protocol

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All solvents
were used directly from the vendor. The 1H-NMR and 13C-NMR spectra were recorded on a JEOL 400
MHz spectrometer (JEOL, Ltd., Tokyo, Japan); at room temperature in
CDCl3 and/or DMSO-d6 using
an internal standard, δ values were expressed in ppm. Elemental
analyses were performed on PerkinElmer 2400 elemental analyzer (PerkinElmer,
Inc. 940 Winter Street, Waltham, MA). Melting points were recorded
on a Gallenkamp melting point apparatus (Sigma-Aldrich Chemie GmbH,
82024 Taufkirchen, Germany) and are uncorrected.
Al Rasheed H., Dahlous K., Sharma A., Sholkamy E., El-Faham A., de la Torre B.G, & Albericio F. (2020). Barbiturate- and Thiobarbituarte-Based s-Triazine Hydrazone Derivatives with Promising Antiproliferative Activities. ACS Omega, 5(26), 15805-15811.
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9

Purification and Characterization of Organic Compounds

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All the chemicals were used as received unless otherwise stated. Diethyl ether (Et2O), tetrahydrofuran (THF), methylene chloride (DCM), and toluene were dried over a column of molecular sieves under argon. All reactions were carried out under an inert nitrogen atmosphere unless otherwise stated. Crude products were purified in a Biotage Isolera One Flash Purification System using Biotage prepacked cartridges (50 μm irregular silica). Yields refer to isolated material following silica gel chromatography. The purity of the compounds tested was determined by quantitative 1H NMR using the absolute internal calibrant method (see the Supporting Information). 1H NMR and 13C NMR spectra were recorded on a JEOL 400 MHz spectrometer using CDCl3 and dimethyl sulfoxide-d6 (DMSO-d6) as the deuterated solvent [≥99.8 atom % D, contains 0.03% (v/v) TMS]. The chemical shifts (δ) were reported in parts per million (ppm) relative to the internal standard TMS. High-resolution mass spectroscopy (HRMS) data were obtained on a UHR-TOF maXis 4G instrument (Bruker Daltonics, Bremen, Germany) using electrospray ionization (ESI). Melting points (mp) were taken in open capillaries on a Stuart melting point apparatus SMP11 and are uncorrected.
Fulo H.F., Shoeib A., Cabanlong C.V., Williams A.H., Zhan C.G., Prather P.L, & Dudley G.B. (2021). Synthesis, Molecular Pharmacology, and Structure–Activity Relationships of 3-(Indanoyl)indoles as Selective Cannabinoid Type 2 Receptor Antagonists. Journal of medicinal chemistry, 64(9), 6381-6396.
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10

NMR Analysis of Organic Compounds

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All NMR studies were carried out on Bruker AVANCE 500 MHz and JEOL 400 MHz spectrometer at 278 K. Compound concentrations were in the range 1–10 mM. Before recording the spectra the required sample was taken in an eppendorf and dissolved in 0.5 mL of either CDCl3 or DMSO-d6 and then transferred to the NMR tube to record the spectra.
Das T., Pramanik A, & Haldar D. (2017). On-line Ammonia Sensor and Invisible Security Ink by Fluorescent Zwitterionic Spirocyclic Meisenheimer Complex. Scientific Reports, 7, 40465.
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