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9 protocols using digital ft nmr spectrometer

1

Microwave-assisted Synthesis of Compounds

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All chemicals used in the study were purchased either from Sigma-Aldrich (St. Louis, MO, USA) or Merck KGaA (Darmstadt, Germany), and used without further chemical or biological purification. Microwave syntheses were realized by using a Monowave 300 high-performance microwave reactor (Anton-Paar, Graz, Austria). Melting points of synthesized compounds were determined by using an automatic melting point determination system (MP90 series, Mettler-Toledo, Ohio, OH, USA) and were uncorrected. 1H-NMR and 13C-NMR spectra were recorded in DMSO-d6 by a Bruker digital FT-NMR spectrometer (Bruker Bioscience, MA, USA) at 300 MHz and 75 MHz, respectively. High resolution mass spectrometric studies were performed using an LCMS-IT-TOF system (Shimadzu, Kyoto, Japan). Chemical purities of the compounds were checked by classical TLC applications performed on silica gel 60 F254 (Merck KGaA); LCMS-IT-TOF chromatograms were also used for the same purpose.
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2

Synthesis and Characterization of Organic Compounds

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Chemicals of the Merck (Merck KGaA, Darmstadt, Germany) or Sigma-Aldrich (Sigma-Aldrich Corp., St. Louis, MO, USA) companies were used in the synthesis. The 1H-NMR and 13C-NMR spectra were recorded in DMSO-d6 at 300 MHz and 75 MHz, pespectively, on a digital FT-NMR spectrometer (Bruker Bioscience, Billerica, MA, USA). The NMR spectra signals were defined as a singlet (s), br.s. (broad singlet), doublet (d), triplet (t), double doublet (dd), and multiplet (m). The coupling constants (J) are reported in units of Hertz (Hz). A FT-IR spectrometer (IRAffinity-1S Fourier transform, Shimadzu, Tokyo, Japan) was used to record the IR spectra of the compounds. MS studies were performed on an LCMS-8040 tandem mass system (Shimadzu) and acetonitrile containing 0.1% formic acid was used as solvent. Silica gel 60 F254 by TLC (Merck KGaA) was used to monitor the progress of reactions.
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3

Comprehensive Analytical Characterization of Chemical Compounds

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All chemicals were obtained either from Sigma-Aldrich (Sigma-Aldrich Corp., St. Louis, MO, USA) or Merck (Merck KGaA, Darmstadt, Germany), and used without further chemical purification. Melting points of the compounds were measured by using an automatic melting point determination instrument (MP90, Mettler-Toledo, OH, USA) and were presented as uncorrected. 1H and 13C-NMR spectra were recorded in DMSO-d6 by a Bruker digital FT-NMR spectrometer (Bruker Bioscience, MA, USA) at 300 MHz and 75 MHz, respectively. The IR spectra of the compounds were recorded using an IRAffinity-1S Fourier transform IR (FTIR) spectrometer (Shimadzu, Tokyo, Japan). The HRMS studies were performed on an LCMS-IT-TOF system (Shimadzu, Tokyo, Japan). Chemical purities of the compounds were checked by classical TLC applications, which was performed on a silica gel 60 F254 (Merck KGaA, Darmstadt, Germany).
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4

Synthesis and Characterization of Novel Compounds

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All chemicals were purchased either from Sigma-Aldrich (Sigma-Aldrich Corp., St. Louis, MO, USA) or Merck (Merck KGaA, Darmstadt, Germany) and used without further chemical purification. Melting points of the synthesized compounds were determined by a MP90 digital melting point apparatus (Mettler Toledo, Columbus, OH, USA) and were uncorrected. 1H- and 13C-NMR spectra were recorded in DMSO-d6 by a Bruker digital FT-NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) at 300/75 MHz. The IR spectra were obtained on an IR Prestige-21 spectrophotometer (Shimadzu, Tokyo, Japan). LC-MS-MS studies were performed on a Shimadzu IT-TOF-LC-MS-MS system. The purities of compounds were checked by TLC on silica gel 60 F254 (Merck KGaA).
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5

Synthesis and Characterization of Organic Compounds

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The complete chemicals used in the synthetic process were acquired
from Merck Chemicals (Merck KGaA, Darmstadt, Germany) or Sigma-Aldrich
Chemicals (Sigma-Aldrich Corp., St. Louis, MO, USA). The compounds’
uncorrected melting points were ascertained using an MP90 digital
melting point instrument (Mettler Toledo, OH, USA). A Bruker digital
FT-NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) operating
at 300 and 75 MHz registered the1H- and13C NMR
spectra of the compounds produced in DMSO-d6, respectively. In the NMR spectra, splitting patterns were denoted
as follows: s for singlet, d for doublet, t for triplet, and m for
multiplet. The reported unit of coupling constants (J) was Hertz.
The Shimadzu LC/MSMS system (Shimadzu, Tokyo, Japan) was used to determine
the M + 1 peaks. Using Silica Gel 60 F254 TLC for thin-layer chromatography
(TLC), all reactions were observed.
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6

Synthetic Compound Characterization Protocol

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All of the chemicals used
in the synthetic process were bought from Merck (Darmstadt, Germany)
or Sigma-Aldrich (St. Louis, MO, USA). The MP90 digital melting point
instrument (Mettler Toledo, OH, USA) was used to determine the uncorrected
melting points of the compounds that were obtained. A Bruker digital
FT NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) was used
to record the 1H and 13C NMR spectra of the
produced compounds in DMSO-d6. Splitting
patterns in the NMR spectra were designated as follows: s, singlet;
d, doublet; t, triplet; m, multiplet. Coupling constants (J) are reported in hertz. [M + 1] peaks were determined
using a Shimadzu LC/MSMS system (Shimadzu, Tokyo, Japan). Using silica
gel 60 F254 TLC plates (Merck), thin-layer chromatography
(TLC) was used to monitor each reaction.
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7

Synthesis and Characterization of Organic Compounds

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All chemicals were obtained either from Sigma-Aldrich Corp. (St. Louis, MO, USA) or Merck KGaA (Darmstadt, Germany), and used without further chemical purification. Melting points of the compounds were measured by using an automatic melting point determination instrument (MP90, Mettler-Toledo, Columbus, OH, USA) and were presented as uncorrected. 1H- and 13C-NMR spectra were recorded in DMSO-d6 by a Bruker digital FT-NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) at 300 MHz and 75 MHz, respectively. The IR spectra of the compounds were recorded using an IRAffinity-1S Fourier transform IR (FTIR) spectrometer (Shimadzu, Tokyo, Japan). MS studies were performed on an LCMS-8040 tandem mass system (Shimadzu, Tokyo, Japan). Chemical purities of the compounds were checked by classical TLC applications performed on silica gel 60 F254 (Merck KGaA).
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8

Synthesis and Characterization of Organic Compounds

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All reagents were purchased from commercial suppliers and were used without further purification. Melting points (M.p.) were determined on an Electrothermal 9100 melting point apparatus (Weiss-Gallenkamp, Loughborough, UK) and are uncorrected. IR spectra were recorded on an IRPrestige-21 Fourier Transform Infrared spectrophotometer (Shimadzu, Tokyo, Japan). 1H NMR and 13C NMR spectra were recorded by a Bruker digital FT-NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) in DMSO-d6. Mass spectra were recorded on an Agilent LC-MSD-Trap-SL Mass spectrometer (Agilent Technologies, Palo Alto, CA, USA). Elemental analyses were performed on a Perkin Elmer EAL 240 elemental analyzer (Perkin-Elmer, Norwalk, CT, USA) and the results were within ±0.4% of the theoretical values. Thin Layer Chromatography (TLC) was performed on TLC Silica gel 60 F254 aluminium sheets (Merck, Darmstadt, Germany) to check the purity of the compounds.
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9

Synthesis and Characterization of Novel Organic Compounds

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All chemicals were obtained either from Sigma-Aldrich (Sigma-Aldrich Corp., St. Louis, MO, USA) or Merck (Merck KGaA, Darmstadt, Germany), and used without further purification. Melting points of the compounds were measured by using an automatic melting point determination instrument (MP90, Mettler-Toledo, Columbus, OH, USA) and are uncorrected. 1H- and 13C-NMR spectra were recorded in DMSO-d6 on a Bruker digital FT-NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) at 300 MHz and 75 MHz, respectively. The IR spectra of the compounds were recorded using an IRAffinity-1S Fourier transform IR (FTIR) spectrometer (Shimadzu, Tokyo, Japan). HRMS studies were performed on an LCMS-IT-TOF system (Shimadzu). Chemical purities of the compounds were checked by classical TLC applications performed on silica gel 60 F254 (Merck KGaA).
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