1H and NMR spectral data were recorded in CDCl3 or DMSO-d6 on a 300 or 400 MHz Bruker NMR spectrometer. Column chromatography was conducted on Revelaris flash chromatography system. Reactions were monitored using thin-layer chromatography (TLC) on silica gel plates. HPLC analysis was conducted on an Agilent 1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18, 4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254nm, room temperature) with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution. HPLC-MS was performed on a Gilson 321 HPLC with detection performed by a Gilson 170 DAD and a Finnigan AQA mass spectrometer operating in electrospray ionization mode using a Phenomenex Gemini C18 150x4.6mm column. Compound purity was determined using an Agilent 1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18, 4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254nm, room temperature) with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution. All compounds were >95% pure via LC/MS analysis.
321 hplc
Manufactured by Gilson
The Gilson 321 HPLC is a high-performance liquid chromatography system designed for analytical and preparative applications. It features a reliable and precise solvent delivery system, robust components, and intuitive software control.
Automatically generated - may contain errors
Lab products found in correlation
Aqa mass spectrometer, by Phenomenex (5 mentions)
Nmr spectrometer, by Bruker (5 mentions)
Gemini c18 150x4.6mm column, by Phenomenex (3 mentions)
Agilent 1100 series lc system, by Agilent Technologies (2 mentions)
1200 system, by Agilent Technologies (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
Nicolet is10 spectrometer, by Thermo Fisher Scientific (1 mentions)
Luna c18 column, by Phenomenex (1 mentions)
Chirascan, by Applied Photophysics (1 mentions)
Acquity uplc system, by Waters Corporation (1 mentions)
6 protocols using 321 hplc
1
Spectroscopic and Chromatographic Analysis
2
Synthesis of Thiosemicarbazone Derivative
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The synthesis of the thiosemicarbazone 5 was according to procedures described previously [37 (link)]. Briefly, 1 eq of the acid and 1 eq of the hydrazine were dissolved in anhydrous ethanol and the resulting reaction mixture was refluxed overnight. The acetone was evaporated and the crude reaction mixture purified by column chromatography. 1H and NMR spectral data were recorded in CDCl3 or Acetone-d6 on a 300 MHz Bruker NMR spectrometer. Column chromatography was carried out on Revelaris flash chromatography system. Reactions were monitored using thin-layer chromatography (TLC) on silica gel plates. HPLC analysis was conducted on an Agilent 1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18, 4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254nm, room temperature) with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution. HPLC-MS was performed on a Gilson 321 HPLC with detection performed by a Gilson 170 DAD and a Finnigan AQA mass spectrometer operating in electrospray ionization mode using a Phenomenex Gemini C18 150x4.6mm column. Yield: (0.011 g, 11%). 1H NMR (300 MHz, MeOD): 2.55 (3H,CH3); 7.62–8.51 (6H, m). LCMS–ESI (M+H)+: 245.1.
3
Analytical Characterization of Compounds
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Optical rotations were measured on a Jasco P-1020 polarimeter using a 1 cm cell. ECD spectra were recorded using an Applied Photophysics Chirascan plus a circular dichroism detector. IR spectra were obtained on a Thermo Nicolet iS10 spectrometer. The NMR spectra were obtained on a 600 MHz NMR Bruker system at the NCIRF (National Center for Interuniversity Research Facilities at Seoul National University). The automated HPLC/SPE/HPLC coupling separation was performed on a Sepiatec Sepbox 2D-250 equipped with UV and ELSD detectors. HPLC-MS data were obtained from an Agilent 1200 system connected with 6120 quadrupole MSD equipped with a Phenomenex Luna C18 column (150 × 4.6 mm, 5 μm). Preparative (prep) HPLC was performed by a Gilson 321 HPLC with a UV/VIS-151 detector (210 nm) and a Shodex-RI-101 refractive index detector.
4
Spectroscopic Characterization of Synthetic Compounds
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1H
and 13C
NMR spectral data were recorded in CDCl3 or DMSO-d6 on a 300 or 400 MHz Bruker NMR spectrometer.
Column chromatography was conducted on a Revelaris flash chromatography
system. Reactions were monitored using thin-layer chromatography (TLC)
on silica gel plates. HPLC analysis was conducted on an Agilent 1100
series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18,
4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254 nm, room temperature)
with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution.
HPLC-MS was performed on a Gilson 321 HPLC with detection performed
by a Gilson 170 DAD and a Finnigan AQA mass spectrometer operating
in electrospray ionization mode using a Phenomenex Gemini C18 150
× 4.6 mm column. Compound purity was determined using an Agilent
1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18,
4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254 nm, room temperature)
with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution.
All compounds were >95% pure via LC/MS analysis. Compounds1 –3 and 47 were a generous
donation
from our collaborators, Lilly Research laboratories.1 –3 , 26 , and 27 are
also commercially available. We acquired NMR and LCMS data to confirm
a match to literature reports.
and 13C
NMR spectral data were recorded in CDCl3 or DMSO-d6 on a 300 or 400 MHz Bruker NMR spectrometer.
Column chromatography was conducted on a Revelaris flash chromatography
system. Reactions were monitored using thin-layer chromatography (TLC)
on silica gel plates. HPLC analysis was conducted on an Agilent 1100
series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18,
4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254 nm, room temperature)
with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution.
HPLC-MS was performed on a Gilson 321 HPLC with detection performed
by a Gilson 170 DAD and a Finnigan AQA mass spectrometer operating
in electrospray ionization mode using a Phenomenex Gemini C18 150
× 4.6 mm column. Compound purity was determined using an Agilent
1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18,
4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254 nm, room temperature)
with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution.
All compounds were >95% pure via LC/MS analysis. Compounds
donation
from our collaborators, Lilly Research laboratories.
also commercially available. We acquired NMR and LCMS data to confirm
a match to literature reports.
5
NMR and HPLC Spectroscopic Analysis
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1H and 13C NMR spectral data were recorded in CDCl3 or DMSO-d6 on a 300 or 400 MHz Bruker NMR spectrometer. Column chromatography was conducted on silica gel (100–300 mesh). Reactions were monitored using thin-layer chromatography (TLC) on silica gel plates. HPLC analysis was conducted on an Agilent 1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18, 4.8 mm × 150 mm, 5 μm, 1.0 mL/min, UV 254 nm, room temperature) with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution. HPLCMSwas performed on a Gilson 321 HPLC with detection performed by a Gilson 170 DAD and a Finnigan AQA mass spectrometer operating in electrospray ionisation mode using a Phenomenex Gemini C18 150x4.6 mm column. Purity was determined using a Waters Acquity UPLC system equipped with a BEH C18 1.7 μm 2.1 × 100 mm column.
6
NMR Spectroscopy and HPLC Analysis Protocol
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1H and NMR spectral data were recorded in CDCl3 or Acetone-d6 on a 300 MHz Bruker NMR spectrometer. Column chromatography was conducted on a Revelaris flash chromatography system. Reactions were monitored using thin-layer chromatography (TLC) on silica gel plates. HPLC analysis was conducted on an Agilent 1100 series LC system (Agilent ChemStation Rev.A.10.02; Phenomenex-Luna-C18, 4.8 mm × 150 mm, 5 µm, 1.0 mL/min, UV 254 nm, room temperature) with MeCN/H2O (0.05% TFA or HCOOH buffer) gradient elution. HPLC-MS was performed on a Gilson 321 HPLC with detection performed by a Gilson 170 DAD and a Finnigan AQA mass spectrometer operating in electrospray ionisation mode using a Phenomenex Gemini C18 150 × 4.6 mm column. Compounds 3a , b , c , s , t and u were purchased from ChemBridge Corporation.
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