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Varian 400 mhz spectrometer

Manufactured by Agilent Technologies
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The Varian 400 MHz spectrometer is a nuclear magnetic resonance (NMR) spectrometer designed for analytical and research applications. It operates at a frequency of 400 MHz and is capable of providing high-resolution NMR data for the structural characterization of chemical compounds.

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Lab products found in correlation

Jms 700 mass spectrometer, by JEOL (3 mentions) Silica gel 60 f254, by Merck Group (3 mentions) G2 qtof mass spectrometer, by JEOL (2 mentions) Hplc system, by Waters Corporation (2 mentions) Thomas hoover melting point apparatus, by Thomas Scientific (1 mentions) Jms 700 mstation, by JEOL (1 mentions) Agilent 7890a gc 5975c msd, by Agilent Technologies (1 mentions) Model qp 2010, by Shimadzu (1 mentions) Silica gel 60 f254 plate, by Merck Group (1 mentions) Dionex ultimate 3000 uhplc, by Thermo Fisher Scientific (1 mentions)

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Varian 400 spectrometer 400 MHz spectrometer Varian spectrometers 400 spectrometer Spectrometers

7 protocols using varian 400 mhz spectrometer

1

Characterization of Organic Compounds

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Chemicals
and reagents were purchased from Sigma-Aldrich (St. Louis, MO) and
used without further purification. Thin-layer chromatography (TLC)
was performed on silica gel glass plates (Silica gel, 60 F254, Fluka,
Merck, Darmstadt, Germany). Kieselgel S (silica gel S, 0.063–0.1
mm, Merck, Darmstadt, Germany) was used for column chromatography.
Melting points were measured using the Gallenkamp apparatus (Toledo,
OH). Infrared spectra were collected in KBr pellets using Thermo Nicolet
model 470 FT-IR spectrophotometers (Thermo Scientific, Waltham, MA).
The 1H NMR and 13C NMR spectra were recorded
using a Varian-400 MHz spectrometer (Agilent Technologies, Santa Clara,
CA) using the CDCl3 solvent and tetramethyl silane (TMS)
as the internal reference. Chemical shifts were stated in parts per
million (δ values, ppm). Elemental analysis was performed using
a Leco CHN-600 elemental analyzer (Ontario, Canada). Microwave synthesis
was performed using the CEM microwave system (Matthews).
Al Neyadi S.S., Adem A., Amir N., Ghattas M.A., Abdou I.M, & Salem A.A. (2024). Novel Thiazolidinedione and Rhodanine Derivatives Regulate Glucose Metabolism, Improve Insulin Sensitivity, and Activate the Peroxisome Proliferator-Activated γ Receptor. ACS Omega, 9(5), 5463-5484.
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2

Characterization of Organic Compounds

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The reagents were commercially purchased from Sigma-Aldrich (St. Louis, MO, USA) or TCI (Tokyo, Japan). If necessary, solvents were purified and/or dried prior to use. All anhydrous reactions were carried out under a dry atmosphere of nitrogen. Melting points (m.p.) were measured on Thomas-Hoover melting point apparatus (Thomas Scientific, Swedesboro, NJ, USA) and not corrected. 1H, 13C-NMR and HMBC spectra were measured on a Varian 400 MHz spectrometer (Agilent Technologies, Santa Clara, CA, USA) in DMSO-d6, CDCl3, or (CD3)2CO. Chemical shifts (δ) are in ppm relative to tetramethylsilane, and coupling constants (J) are in Hz. DIP-MS (EI) was measured on an Agilent 7890A-5975C GC/MSD (Agilent Technologies). GC/MS (EI) was determined on a SHIMADZU QP 2010 model (Shimadzu, Kyoto, Japan) and FAB-MS was determined on a JEOL JMS-700 Mstation (JEOL, Tokyo, Japan). Fraction collection was performed on an EYELA fraction collector DC-1500 (Tokyo Rikakikai, Tokyo, Japan). An analytical TLC was performed on pre-coated silica gel 60 F254 plates (Merck, Kenilworth, NJ, USA). Solvent systems for TLC and column chromatography were ethyl acetate/n-hexane mixtures and 10% methanol in dichloromethane. Column chromatography was carried out on Merck silica gel 9385 (Merck).
Lee S.H., Lee W., Nguyen T., Um I.S., Bae J.S, & Ma E. (2017). Synthesis and Thrombin, Factor Xa and U46619 Inhibitory Effects of Non-Amidino and Amidino N2-Thiophenecarbonyl- and N2-Tosylanthranilamides. International Journal of Molecular Sciences, 18(6), 1144.
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3

Synthesis and Characterization of Novel Compounds

Cited 1 time
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In the conducted experiments all acquired solvents and reagents were applied without additional purification. Varian 400 MHz spectrometer (Varian Medical Systems, Inc., Palo Alto, CA, USA) was utilised to calculate the 1H NMR spectra with chemical shifts being measured in parts per million (ppm) and coupling constants in Hz. The high-resolution electrospray ionisation mass spectrometry (HR-ESIMS) data were assessed utilising a JMS–700 mass spectrometer (Jeol, Japan) or by HR-ESIMS data obtained via a G2 QTOF mass spectrometer. Reaction monitoring was carried out using TLC on 0.25 mm silica plates (E. Merck; silica gel 60 F254). Reverse-phase high performance liquid chromatography (RP-HPLC) was employed to determine the purity of the products, with the UV detector of the HPLC being set at 254 nm. The mobile phases employed were: (A) H2O containing 0.05% TFA and (B) CH3CN. The purity of the final compound was determined using a gradient of 75% B or 100% B in 30 min. The melting points were measured using a Fisherbrand digital melting point apparatus. Compounds 2a–b and 3a–d were synthesised as reported earlier34 (link). The final target compounds were synthesised following the reported procedure of Suzuki cross-coupling reaction34 (link).
Nada H., Elkamhawy A., Abdellattif M.H., Angeli A., Lee C.H., Supuran C.T, & Lee K. (2022). 4-Anilinoquinazoline-based benzenesulfonamides as nanomolar inhibitors of carbonic anhydrase isoforms I, II, IX, and XII: design, synthesis, in-vitro, and in-silico biological studies. Journal of Enzyme Inhibition and Medicinal Chemistry, 37(1), 994-1004.
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4

Analytical Characterization of Chemical Compounds

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The experiments were carried
out by using the purchased reagents and solvents without further purification.
The 1H NMR spectra were captured by using a Varian 400 MHz spectrometer
(Varian Medical Systems, Inc., Palo Alto, CA, USA), with chemical
shifts being recorded in parts per million (ppm) and coupling constants
in Hz. HR electrospray ionization (ESI) MS data were collected using
either a G2 QTOF mass spectrometer or a JMS-700 mass spectrometer
(both from Jeol, Japan). Thin-layer chromatography was employed to
monitor the reactions on 0.25 mm silica plates (E. Merck; silica gel
60 F254). Using an HPLC system from Waters Corp. with a UV detector
set at 254 nm, reversed-phase HPLC was used to assess the purity of
the products. Both A and B, which were mobile phases, contained 0.05%
TFA in water. HPLC was used with a YMC Hydrosphere C18 (HS-302) column
that was 4.6 mm in diameter and 150 mm in length and had a flow rate
of 1.0 mL/min. The column had a 5 M particle size and a 12 nm pore
size. Using either a gradient of 75% B or 100% B in 30 min, the resulting
compounds’ purity was determined. To measure the melting points,
a Fisherbrand digital melting point instrument was employed.
Nada H., Gul A.R., Elkamhawy A., Kim S., Kim M., Choi Y., Park T.J, & Lee K. (2023). Machine Learning-Based Approach to Developing Potent EGFR Inhibitors for Breast Cancer—Design, Synthesis, and In Vitro Evaluation. ACS Omega, 8(35), 31784-31800.
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5

Analytical Characterization of Organic Compounds

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All solvents and reagents
were used without further purification. A Varian 400 MHz spectrometer
(Varian Medical Systems, Inc., Palo Alto, CA) was used to calculate
the 1H NMR spectra with chemical shifts and coupling constants
measured in ppm (parts per million) and Hz, respectively. HR-ESIMS
data were analyzed with a JMS-700 mass spectrometer or G2 QTOF mass
spectrometer. Reaction observation was performed using TLC on 0.25
mm silica plates (E. Merck; silica gel 60 F254). Reversed-phase high-performance
liquid chromatography (RP-HPLC) with a UV detector set at 254 nm was
used to test the purity of the products. Mobile phases included H2O with 0.05% TFA and CH3CN, and a gradient of 75%
B or 100% B was used for 45 min. Melting points were measured with
a Fisher brand digital melting point instrument to determine the purity
of the final product.
Nada H., Kim S., Park S., Lee M.Y, & Lee K. (2023). Identification of Potent hDHODH Inhibitors for Lung Cancer via Virtual Screening of a Rationally Designed Small Combinatorial Library. ACS Omega, 8(24), 21769-21780.
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6

Analytical Characterization of Organic Compounds

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The purchased solvents and reagents were used without further purification in the conducted experiments. Varian 400 MHz spectrometer (Varian Medical Systems, Inc., Palo Alto, CA, USA) was used to record the 1H NMR spectra with chemical shifts being recorded in parts per million (ppm) and coupling constants in Hz, as reported previously [49 (link)]. The high-resolution electrospray ionization mass spectrometry (HR-ESIMS) data were recorded on a JMS-700 mass spectrometer (Jeol, Japan) or by HR-ESIMS data recorded on a G2 QTOF mass spectrometer (Thermo Scientific™, Waltham, MA, USA). The reactions were monitored using TLC on 0.25 mm silica plates (E. Merck, Darmstadt, Germany; silica gel 60 F254). The purity of the products was determined by reversed-phase high performance liquid chromatography (RP-HPLC) utilizing Waters Corp. HPLC system equipped with a UV detector set at 254 nm (Milford, MA, USA). The mobile phases used were: (A) H2O containing 0.05% TFA and (B) CH3CN. HPLC employed a YMC Hydrosphere C18 (HS-302) column (5 μM particle size, 12 nm pore size) that was 4.6 mm in diameter × 150 mm in size, with a flow rate of 1.0 mL/min. The final compounds purity was assessed using either a gradient of 75% B or 100% B in 30 min. A Fisherbrand digital melting point apparatus was used to measure the melting points.
Lee K., Nada H., Byun H.J., Lee C.H, & Elkamhawy A. (2021). Hit Identification of a Novel Quinazoline Sulfonamide as a Promising EphB3 Inhibitor: Design, Virtual Combinatorial Library, Synthesis, Biological Evaluation, and Docking Simulation Studies. Pharmaceuticals, 14(12), 1247.
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7

NMR and Spectroscopic Analysis of Organic Compounds

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Nuclear magnetic resonance (NMR) spectroscopy data were recorded on a Varian 400 MHz spectrometer (400 and 100 MHz, respectively, Varian, Palo Alto, CA, USA). Chemical shifts are referenced to solvent (7.26 and 77.00 ppm for CDCl3 and 7.16 and 128.36 ppm for benzene-d6). The data are depicted in the Results and Discussion sections. Additional data: IR (ATR): 2970 (w); ~2950 (br) (OH); 2911 (w); 2856 (m); 1722 (w); 1640 (s) (C=O); 1568 (s); 1450 (s); 1404 (m); 1262 (s); 1190 (s); 1137 (m); 780 (m); 733 (s) cm−1 obtained on a Bruker ALPHA Platinum ATR A220/D-OX (Bruker, Billerica, MA, USA); MS (ESI-) m/z (%): 540.17, calculated for C32H28O8: 540.1784 (Dionex Ultimate 3000 UHPLC, Thermo, San José, CA, USA).
Kretschmer N., Durchschein C., Hufner A., Rinner B., Lohberger B, & Bauer R. (2022). SK119, a Novel Shikonin Derivative, Leads to Apoptosis in Melanoma Cell Lines and Exhibits Synergistic Effects with Vemurafenib and Cobimetinib. International Journal of Molecular Sciences, 23(10), 5684.
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