An Agilent Technologies LC/MSD TOF instrument was used to record the high-resolution mass spectra. Varian Mercury 400 and 100 MHz spectrometers were used to record the 1H and 13C NMR spectra. High-performance liquid chromatography (HPLC, Shimadzu LC-20A) with a reverse-phase C18 column (4.6 mm × 150 mm, 5 mm, Shim-pack VP-ODS) was used to determine the purity of the target compounds (all above 95%). The detailed chemical data, the 1H and 13C NMR spectra, and the high-resolution mass spectra are provided in the Supplementary material .
Lc msd tof instrument
Manufactured by Agilent Technologies
The LC/MSD TOF instrument is a liquid chromatography-mass spectrometry (LC-MS) system designed for high-resolution, accurate-mass detection. It combines liquid chromatography (LC) with time-of-flight mass spectrometry (TOF-MS) to provide precise molecular mass information for chemical analysis.
Automatically generated - may contain errors
Lab products found in correlation
Drx 600, by Bruker (3 mentions)
Drx 500, by Bruker (2 mentions)
Lc 20a, by Shimadzu (1 mentions)
Mercury 400, by Agilent Technologies (1 mentions)
Vp ods, by Shimadzu (1 mentions)
Drx 300, by Bruker (1 mentions)
Drx 400, by Bruker (1 mentions)
Mercury 400 spectrometer, by Agilent Technologies (1 mentions)
Avance 3, by Bruker (1 mentions)
Gf254, by Merck Group (1 mentions)
7 protocols using lc msd tof instrument
1
Analytical Characterization of Compounds
2
Synthesis and characterization of novel compounds
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All compounds were fully characterized
by spectroscopic data. The NMR spectra were recorded on a Bruker DRX500
or DRX600. Chemical shifts (δ) are expressed in parts per million, J values are given in hertz, and deuterated dimethyl sulfoxide
(DMSO)-d6 or CDCl3 was used
as a solvent. IR spectra were recorded on an FTIR Thermo Nicolet Avatar
360 using a KBr pellet. The reactions were monitored by thin-layer
chromatography (TLC) using silica gel GF254. The melting
points were determined on an XT-4A melting point apparatus and were
uncorrected. HRMS were performed on an Agilent LC/MSD TOF instrument.
X-ray diffraction was carried out by APEX DUO.
All chemicals
and solvents were used as received without further purification unless
otherwise stated. All chemicals were purchased from Adamas-β.
Column chromatography was performed on silica gel (Qingdao, 200–300
mesh). Compounds1 were prepared according to the literature.50 (link),51 (link)
by spectroscopic data. The NMR spectra were recorded on a Bruker DRX500
or DRX600. Chemical shifts (δ) are expressed in parts per million, J values are given in hertz, and deuterated dimethyl sulfoxide
(DMSO)-d6 or CDCl3 was used
as a solvent. IR spectra were recorded on an FTIR Thermo Nicolet Avatar
360 using a KBr pellet. The reactions were monitored by thin-layer
chromatography (TLC) using silica gel GF254. The melting
points were determined on an XT-4A melting point apparatus and were
uncorrected. HRMS were performed on an Agilent LC/MSD TOF instrument.
X-ray diffraction was carried out by APEX DUO.
All chemicals
and solvents were used as received without further purification unless
otherwise stated. All chemicals were purchased from Adamas-β.
Column chromatography was performed on silica gel (Qingdao, 200–300
mesh). Compounds
3
Synthesis and Characterization of Heterocyclic Ketene Acetals
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All received reagents and solvents
were used without further purification unless otherwise stated. Melting
points were determined on an XT-4A melting point apparatus and were
uncorrected. NMR spectra were recorded on Bruker DRX300 (1H: 300 MHz, 13C: 75 MHz), Bruker DRX400 (1H:
400 MHz, 13C: 100 MHz), Bruker DRX500 (1H: 500
MHz, 13C: 125 MHz), and Bruker DRX600 (1H: 600
MHz, 13C: 150 MHz) instruments with DMSO-d6 and CDCl3 as the solvents. The chemical shifts
(δ) are expressed in parts per million relative to the residual
deuterated solvent signal, and coupling constants (J) are given in hertz. IR spectra were recorded on an FT-IR Thermo
Nicolet Avatar 360 instrument using KBr pellets. HRMS (electrospray
ionization) was performed on an Agilent LC/MSD TOF instrument.
All received reagents and solvents were used without further purification
unless otherwise stated. The materials (1a–d )
were purchased from Aldrich Corporation Limited. HKAs2 were prepared according to a procedure described in the literature.39 (link),40 (link) The structure of HKAs 2 was confirmed by 1H NMR, 13C NMR, and HRMS spectra.
were used without further purification unless otherwise stated. Melting
points were determined on an XT-4A melting point apparatus and were
uncorrected. NMR spectra were recorded on Bruker DRX300 (1H: 300 MHz, 13C: 75 MHz), Bruker DRX400 (1H:
400 MHz, 13C: 100 MHz), Bruker DRX500 (1H: 500
MHz, 13C: 125 MHz), and Bruker DRX600 (1H: 600
MHz, 13C: 150 MHz) instruments with DMSO-d6 and CDCl3 as the solvents. The chemical shifts
(δ) are expressed in parts per million relative to the residual
deuterated solvent signal, and coupling constants (J) are given in hertz. IR spectra were recorded on an FT-IR Thermo
Nicolet Avatar 360 instrument using KBr pellets. HRMS (electrospray
ionization) was performed on an Agilent LC/MSD TOF instrument.
All received reagents and solvents were used without further purification
unless otherwise stated. The materials (
were purchased from Aldrich Corporation Limited. HKAs
4
Diarylmethyl Sulfone Synthesis
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All received reagents and solvents
were used without further purification, unless otherwise stated. Melting
points were determined on a XT-4A melting point apparatus and are
uncorrected. NMR spectra were recorded on a Bruker 400 (1H: 400 MHz, 13C: 100 MHz) with CDCl3 as the
solvent. The chemical shifts (δ) are expressed in parts per
million relative to the residual deuterated solvent signal, and coupling
constants (J) are given in hertz. HRMS (electrospray
ionization) was performed on an Agilent LC/MSD TOF instrument.
All chemicals and solvents were used as received without further
purification, unless otherwise noted. Column chromatography was performed
on silica gel (200–300 mesh). p-QMs2 and sulfonyl hydrazides 3 were prepared according
to a procedure described in the literature.9 (link),37 (link)−39 (link),41 (link) The structure of diarylmethyl
sulfones4 were confirmed by 1H NMR, 13C NMR, and HRMS spectra.
were used without further purification, unless otherwise stated. Melting
points were determined on a XT-4A melting point apparatus and are
uncorrected. NMR spectra were recorded on a Bruker 400 (1H: 400 MHz, 13C: 100 MHz) with CDCl3 as the
solvent. The chemical shifts (δ) are expressed in parts per
million relative to the residual deuterated solvent signal, and coupling
constants (J) are given in hertz. HRMS (electrospray
ionization) was performed on an Agilent LC/MSD TOF instrument.
All chemicals and solvents were used as received without further
purification, unless otherwise noted. Column chromatography was performed
on silica gel (200–300 mesh). p-QMs
to a procedure described in the literature.9 (link),37 (link)−39 (link),41 (link) The structure of diarylmethyl
sulfones
5
Synthesis and Characterization of Piperazine Derivative
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All chemicals were commercially available without further purification. 1H NMR spectra were recorded on the Varian Mercury 400 spectrometer (Figure S1
Compounds 2–4 were synthesized by the reported method.17 (link) Compound 4 (1 mmol) and 1-[(4-methylphenyl) carbonyl] piperazine (1mmol) were added to a solution of acid derivatives (1.2 mmol) in toluene (10 mL). The mixture was refluxed for 8 h. After evaporation, the crude product was purified by flash column chromatography to afford wyc-7-20. Yield: 88%; 1H NMR (400 MHz, CDCl3) δ 9.33 (s, 1H), 8.76 (d, J = 3.6 Hz, 1H), 8.38 (dt, J = 8.0, 1.9 Hz, 1H), 7.48–7.42 (m, 1H), 7.32–7.28 (m, 2H), 7.23–7.18 (m, 2H), 4.00 (s, 2H), 3.70 (d, J = 98.6 Hz, 4H), 2.70 (s, 4H), 2.37 (s, 3H); HR-ESI-MS: m/z calcd for C20H22N5O2+ 364.1773 ([M+H]+), found 364.1776.
Compounds 2–4 were synthesized by the reported method.17 (link) Compound 4 (1 mmol) and 1-[(4-methylphenyl) carbonyl] piperazine (1mmol) were added to a solution of acid derivatives (1.2 mmol) in toluene (10 mL). The mixture was refluxed for 8 h. After evaporation, the crude product was purified by flash column chromatography to afford wyc-7-20. Yield: 88%; 1H NMR (400 MHz, CDCl3) δ 9.33 (s, 1H), 8.76 (d, J = 3.6 Hz, 1H), 8.38 (dt, J = 8.0, 1.9 Hz, 1H), 7.48–7.42 (m, 1H), 7.32–7.28 (m, 2H), 7.23–7.18 (m, 2H), 4.00 (s, 2H), 3.70 (d, J = 98.6 Hz, 4H), 2.70 (s, 4H), 2.37 (s, 3H); HR-ESI-MS: m/z calcd for C20H22N5O2+ 364.1773 ([M+H]+), found 364.1776.
6
Detailed Characterization of Organic Compounds
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All reagents were obtained from commercial
suppliers and used without further purification. All compounds were
characterized by full spectroscopic data. The 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded
on Bruker Avance III 400 MHz (1H NMR: 400 MHz, 13C NMR: 100 MHz) using CDCl3, DMSO-d6, and F3CCOOD as solvents with tetramethylsilane
as the internal standard (when CDCl3, DMSO-d6, and so forth were unable to dissolve the product, we
chose F3CCOOD as a solvent). Chemical shifts are given
in ppm (δ) referenced to CDCl3 with 7.26 for 1H and 77.16 for 13C, DMSO-d6 with 2.50 for 1H and 39.52 for 13C,
and F3COOD with 11.50 for 1H and 164.2 for 13C. The signals are abbreviated as follows: s, singlet; d,
doublet; t, triplet; q, quartet; and m, multiplet, and the coupling
constants are expressed in hertz. The melting points were determined
on a Tech X-5 melting point apparatus and are uncorrected. IR spectra
(KBr pellet) were detected by a Thermo Nicolet S10 Fourier transform
infrared (FTIR) instrument. High-resolution mass spectrometry (HRMS)
measurements were performed on an Agilent LC/MSD TOF instrument. X-ray
crystallography patterns were obtained from a TTRAX III X-ray diffractometer.
suppliers and used without further purification. All compounds were
characterized by full spectroscopic data. The 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded
on Bruker Avance III 400 MHz (1H NMR: 400 MHz, 13C NMR: 100 MHz) using CDCl3, DMSO-d6, and F3CCOOD as solvents with tetramethylsilane
as the internal standard (when CDCl3, DMSO-d6, and so forth were unable to dissolve the product, we
chose F3CCOOD as a solvent). Chemical shifts are given
in ppm (δ) referenced to CDCl3 with 7.26 for 1H and 77.16 for 13C, DMSO-d6 with 2.50 for 1H and 39.52 for 13C,
and F3COOD with 11.50 for 1H and 164.2 for 13C. The signals are abbreviated as follows: s, singlet; d,
doublet; t, triplet; q, quartet; and m, multiplet, and the coupling
constants are expressed in hertz. The melting points were determined
on a Tech X-5 melting point apparatus and are uncorrected. IR spectra
(KBr pellet) were detected by a Thermo Nicolet S10 Fourier transform
infrared (FTIR) instrument. High-resolution mass spectrometry (HRMS)
measurements were performed on an Agilent LC/MSD TOF instrument. X-ray
crystallography patterns were obtained from a TTRAX III X-ray diffractometer.
7
Characterization of Organic Compounds
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All reagents used were commercially obtained. Reactions were monitored by thin-layer chromatography (TLC) on glass plates coated with silica gel using a fluorescent indicator (GF254, Merck, Germany). The NMR spectral data were recorded on Bruker DRX-600 (1H: 600 MHz, 13C: 151 MHz), respectively. HRMS was performed on an Agilent LC/MSD TOF instrument. All chemical reagents were purchased from Aladdin and Macklin.
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