All melting points were uncorrected. The progression of all the reactions was monitored by thin layer chromatography (TLC) using hexanes/ethyl acetate mixture as eluent. Column chromatography was carried out on silica gel by using increasing polarity. 1H, 13C and DEPT-135 spectra were recorded in CDCl3 using TMS as an internal standard on a Bruker 300 MHz spectrometer at room temperature. Chemical shift values were quoted in parts per million (ppm) and coupling constants (J) were quoted in Hertz (Hz). Mass spectra were recorded on JEOL GC mate mass spectrometer. The X-ray diffraction measurements were carried out at 298 K on a Bruker (2008) SMART APEX 2 area detector diffractometer (S1 File ).
300 mhz spectrometer
Manufactured by Bruker
Sourced in United States, Germany, Italy
The 300 MHz spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It operates at a frequency of 300 MHz, which is a common frequency used for the analysis of organic compounds and biomolecules. The spectrometer provides a high-resolution spectrum that can be used to identify and characterize the chemical structure of samples.
Automatically generated - may contain errors
Lab products found in correlation
500 mhz spectrometer, by Bruker (5 mentions)
400 mhz spectrometer, by Bruker (4 mentions)
Rf 5301pc spectrophotofluorimeter, by Shimadzu (3 mentions)
Mestrenova, by Mestrelab Research (2 mentions)
8453 spectrometer, by Agilent Technologies (2 mentions)
Gcms qp2020 gas chromatograph mass spectrometer, by Shimadzu (2 mentions)
Sta449f3, by Netzsch (2 mentions)
Lcms it tof unit, by Shimadzu (2 mentions)
Glutamine, by Merck Group (2 mentions)
Single beam uv vis spectrophotometer, by Agilent Technologies (2 mentions)
Creatinine, by Merck Group (2 mentions)
Ascorbic acid, by Merck Group (2 mentions)
Smart apex2 area detector diffractometer, by Bruker (1 mentions)
Gcmate mass spectrometer, by JEOL (1 mentions)
Ft ir 1600 spectrophotometer, by PerkinElmer (1 mentions)
Spectrum rx1 spectrophotometer, by PerkinElmer (1 mentions)
Jem 2100, by JEOL (1 mentions)
Gcms qp2010, by Shimadzu (1 mentions)
Dsq 2, by Thermo Fisher Scientific (1 mentions)
Flash 2000, by Thermo Fisher Scientific (1 mentions)
92 protocols using 300 mhz spectrometer
1
Synthesis and Characterization of Novel Compounds
2
Characterization of Organic Compounds
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All reagents were purchased from Aldrich and were used as received. All solvents were dried before use. 1H NMR (300.13185 MHz) and 13C NMR (75.47564 MHz) analyses in CDCl3 were performed on a Bruker 300 MHz spectrometer, using TMS as the internal reference. Chemical shifts (δ) are reported in p.p.m. IR spectra were recorded on a Perkin–Elmer FT–IR 1600 spectrophotometer in the 4000–400 cm−1 range. Elemental analyses were performed in a Thermofinniga Flash 112 instrument under standard conditions.
3
Characterization of Polymer Nanoparticles
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The particle size and particle size distribution (PSD) of the latex were measured using a dynamic light scattering technique (DLS, Nanotrac 150 particle size analyzer, Pittsburgh, PA, USA, range: 0.8–6500 nm, angle: 180 deg) and reported as the number-average diameter (Dn).
The chemical structures of the macro-RAFT agent and PIP-co-RAFT nanoparticles were determined by 1H Nuclear magnetic resonance (NMR) spectroscopy (Bruker 300 MHz spectrometer, Billerica, MA, USA). The sample solution was prepared by dissolving 20 mg of the macro-RAFT agent and PIP-co-RAFT-SiO2 nanoparticles in 1 mL of deuterium oxide (D2O) and deuterated chloroform (CDCl3), respectively.
The VTS-SiO2 and PIP-co-RAFT-SiO2 nanoparticles were characterized by Fourier-transform infrared (FTIR) spectroscopy (Perkin Elmer Spectrum RX I spectrophotometer, Waltham, MA, USA). Infrared spectra were recorded in the region 4000–500 cm−1, with a resolution of 0.5 cm−1.
The morphology of PIP-co-RAFT and PIP-co-RAFT-SiO2 nanoparticles were examined using a transmission electron microscope (TEM, JEOL JEM-2100, Peabody, MA, USA) operating at an acceleration voltage of 80 kV. The latex sample diluted 20 times with deionized water was dropped on a 400-mesh copper grid at room temperature and the grid was stained with 1% OsO4 prior to analysis to obtain sufficient contrast.
The chemical structures of the macro-RAFT agent and PIP-co-RAFT nanoparticles were determined by 1H Nuclear magnetic resonance (NMR) spectroscopy (Bruker 300 MHz spectrometer, Billerica, MA, USA). The sample solution was prepared by dissolving 20 mg of the macro-RAFT agent and PIP-co-RAFT-SiO2 nanoparticles in 1 mL of deuterium oxide (D2O) and deuterated chloroform (CDCl3), respectively.
The VTS-SiO2 and PIP-co-RAFT-SiO2 nanoparticles were characterized by Fourier-transform infrared (FTIR) spectroscopy (Perkin Elmer Spectrum RX I spectrophotometer, Waltham, MA, USA). Infrared spectra were recorded in the region 4000–500 cm−1, with a resolution of 0.5 cm−1.
The morphology of PIP-co-RAFT and PIP-co-RAFT-SiO2 nanoparticles were examined using a transmission electron microscope (TEM, JEOL JEM-2100, Peabody, MA, USA) operating at an acceleration voltage of 80 kV. The latex sample diluted 20 times with deionized water was dropped on a 400-mesh copper grid at room temperature and the grid was stained with 1% OsO4 prior to analysis to obtain sufficient contrast.
4
Characterization of Isolated Compounds
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Isolated compounds HR1–HR5 were characterized
by 1H and 13C nuclear magnetic resonance (1H
and 13C NMR) spectroscopy on Bruker 300 MHz, spectrometer, utilizing
internal standards such as TMS at Quaid-e-Azam University, Islamabad,
and gas chromatography–mass spectrometry(GC–MS) on GCMS-QP 2010 (Shimadzu, JAPAN) at Government College University,
Lahore to elucidate their chemical structures.
by 1H and 13C nuclear magnetic resonance (1H
and 13C NMR) spectroscopy on Bruker 300 MHz, spectrometer, utilizing
internal standards such as TMS at Quaid-e-Azam University, Islamabad,
and gas chromatography–mass spectrometry
Lahore to elucidate their chemical structures.
5
Detailed Compound Characterization Protocol
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Completion of
the reactions and purity of the compounds were monitored
by thin layer chromatography (TLC) on silica gel plates (60 F254; Merck), visualizing with iodine vapors. A Veego make silicon
oil bath-type melting point apparatus was used to determine the melting
points and are uncorrected. The IR spectra were recorded using attenuated
total reflectance and KBr disc methods for liquid and solid samples,
respectively, on a Bruker FT-IR spectrometer, model alpha. The PMR
spectra were recorded using a Bruker 300 MHz spectrometer in deuterated
solvents (CDCl3 and DMSO-d6) (chemical shifts in δ ppm; s is used for a singlet; m, for
a multiplet; t, for a triplet; bs, for a broad singlet; bm, for a
broad multiplet; and bt, for a broad triplet). Mass spectral data
were obtained on a scientific mass spectrometer (Thermo, DSQ II).
Elemental analyses were performed on a Thermo Fisher FLASH 2000 organic
elemental analyzer. All of the final GAs offered results within ±0.4%
of the calculated values of carbon, hydrogen, and nitrogen elements.
the reactions and purity of the compounds were monitored
by thin layer chromatography (TLC) on silica gel plates (60 F254; Merck), visualizing with iodine vapors. A Veego make silicon
oil bath-type melting point apparatus was used to determine the melting
points and are uncorrected. The IR spectra were recorded using attenuated
total reflectance and KBr disc methods for liquid and solid samples,
respectively, on a Bruker FT-IR spectrometer, model alpha. The PMR
spectra were recorded using a Bruker 300 MHz spectrometer in deuterated
solvents (CDCl3 and DMSO-d6) (chemical shifts in δ ppm; s is used for a singlet; m, for
a multiplet; t, for a triplet; bs, for a broad singlet; bm, for a
broad multiplet; and bt, for a broad triplet). Mass spectral data
were obtained on a scientific mass spectrometer (Thermo, DSQ II).
Elemental analyses were performed on a Thermo Fisher FLASH 2000 organic
elemental analyzer. All of the final GAs offered results within ±0.4%
of the calculated values of carbon, hydrogen, and nitrogen elements.
6
NMR Characterization of Synthetic Compounds
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Approx. 5 mg of the small molecule, that is, the synthesized functionals
shown inScheme 1 ,
were dissolved in 600 μL of CDCl3, and the solution
was transferred into 5 mm NMR tubes. The spectra were acquired on
a Bruker 300 MHz spectrometer or on a Bruker 400 MHz spectrometer
using 64 scans at 20 °C within the standard zg pulse sequence.
NMR data were processed with MestreNova (Version 8.1.1, Mestrelab
Research).
shown in
were dissolved in 600 μL of CDCl3, and the solution
was transferred into 5 mm NMR tubes. The spectra were acquired on
a Bruker 300 MHz spectrometer or on a Bruker 400 MHz spectrometer
using 64 scans at 20 °C within the standard zg pulse sequence.
NMR data were processed with MestreNova (Version 8.1.1, Mestrelab
Research).
7
Synthesis and Characterization of Novel Compounds
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Melting points were recorded using a digital Gallenkamp (SANYO) model MPD 350 apparatus and are uncorrected. FTIR spectra were recorded using an FTS 3000 MX spectrophotometer; the 1H NMR and 13C NMR spectra (DMSO-d6) were recorded using a Bruker 300 MHz spectrometer. Chemical shifts (δ) are reported in ppm downfield from the internal standard tetramethylsilane (TMS). Mass spectra were performed on an Agilent 6460 Series Triple Quadrupole instrument (Agilent). The ionization was achieved by electrospray ionization in the positive ion mode (ESI+) and negative ion mode (ESI-). The capillary voltage was set to 4.0 kV. The source temperature was 120°C, and the desolvation temperature was 350°C. Nitrogen was used as a desolvation gas (flow 600 L/h). The software used for in-silico molecular docking studies are AutoDock Tools 1.5.6: La Jolla, CA, U.S.A., AutoDock Vina 1.1.2: La Jolla, CA, U.S.A. and Discovery Studio 4.0: San Diego, CA, U.S.A. The procedure for the synthesis of the desired compounds is depicted in Scheme I. ATP, L-alanine, AMP-PCP and bovine serum albumin (BSA) were purchased from Sigma. Malachite green phosphate detection reagent, UNAM, and E. coli MurC were prepared as described previously [22 (link)].
8
NMR Characterization of Ionic Liquid Decomposition
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A Bruker 300 MHz spectrometer was used to measure 1H NMR spectra. Approximately 6 mg of each sample was digested in 0.7 mL of a stock solution of DCl (20%)/D2O (0.889 mL) and DMSO-d6 (3 mL). Data analysis was performed in TopSpin software. Predicted 1H NMR spectra of decomposed IL structures was generated using www.nmrdb.org after drawing the corresponding chemical structure of decomposed EMIM cations67 (link),68 (link).
9
Comprehensive Analytical Characterization of Toxicant Metabolites
10
Quantitative 31P NMR Analysis of Organosolv Lignin
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Hydroxyl content analysis was performed using a quantitative 31P NMR procedure as published elsewhere [19 (link)]. Spectra were acquired using a Bruker 300 MHz spectrometer equipped with a quad probe at the Institute for Macromolecular Chemistry (University of Freiburg, Freiburg, Germany). An exact amount of 25−30 mg of the organosolv lignin samples was diluted in 400 μL of CDCl3/pyridine (1:1.6) and 150 μL of a solution of chromium(III) acetylacetonate (3.6 mg/mL) as a relaxation agent and cyclohexanol (4.0 mg/mL) as an internal standard in CDCl3/pyridine (1:1.6) was added and the solution was stirred for 5 min. 2-Chloro-4,4,5,5-tetramethyl-1,2,3-dioxaphospholane (TMDP, 70 μL) was then added, and the solution was transferred into an NMR tube for analyzing 31P NMR spectra with 128 scans and a delay time of 15 s.
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