Column chromatography were proceeded with Silica gel 60 F254 (70–230; Merck; Darmstadt, Germany). TLC developed on precoated silica gel Kieselgel 60 F254 plates (0.25 mm thick) and compounds were detected by spraying with 50% H2SO4 on it before being heated at 100 °C. Semi-preparative and preparative HPLC was performed using a Gilson FX-281322H2 High Performance Liquid Chromatography coupled to a DAD detector and an automatic fraction collector. ASunfire C18 column (10 μm, 10 × 250 mm) and (5 μm, 10 × 150 mm) were used in these separations. (+)-ESITOF-MS was performed as previously described [12 ]. We recorded NMR spectra on a Bruker Avance III spectrometer, equipped with a 1.7 mm TCI microcryoprobe, (500.0 and 125.0 MHz for 1H and 13C NMR, respectively). The chemical shifts are given in part per million (ppm) using the signal of the residual solvent as internal reference. The coupling constant (J) are in Hertz.
Tci microcryoprobe
Manufactured by Bruker
Sourced in Switzerland
The TCI MicroCryoProbeTM is a cryogenic NMR probe designed for high-sensitivity and high-resolution nuclear magnetic resonance (NMR) spectroscopy. It features a miniaturized sample coil and a low-temperature environment to enhance signal detection and spectral quality.
Automatically generated - may contain errors
Lab products found in correlation
Avance 3 spectrometer, by Bruker (8 mentions)
P 2000 polarimeter, by Jasco (6 mentions)
Agilent 1100 dad, by Agilent Technologies (5 mentions)
Ft ir 4100 spectrometer, by Jasco (5 mentions)
Maxis q tof spectrometer, by Bruker (2 mentions)
Acquity uplc equipment, by Waters Corporation (2 mentions)
Beh c18 column, by Waters Corporation (2 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Maxis q tof, by Bruker (1 mentions)
Agilent 1200 lc, by Agilent Technologies (1 mentions)
Genesys 10, by Thermo Fisher Scientific (1 mentions)
Maxis q tof mass spectrometer, by Bruker (1 mentions)
Agilent 1260 infinity 2, by Agilent Technologies (1 mentions)
Sunfire c18 column, by Waters Corporation (1 mentions)
Alliance chromatographic system, by Waters Corporation (1 mentions)
Atlantis c18 column, by Waters Corporation (1 mentions)
9 protocols using tci microcryoprobe
1
Purification and Characterization of Compounds
2
Spectroscopic Analysis of Chemical Compounds
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UV spectra were acquired
on a Thermo Fisher Scientific Genesys 10S. Infrared (IR) spectra were
taken on film in a KBr window on a Perkin Elmer 500 series FTIR Panagon
1000. 1D and 2D NMR spectra were recorded on a Bruker AVANCE III spectrometer
at 500/125 MHz (1H/13C NMR, respectively) equipped
with a 1.7 mm TCI MicroCryoProbe (Bruker Biospin, Fällanden,
Switzerland). All shifts are given in δ (ppm) using the signal
of tetramethylsilane as reference. All coupling constants (J) are given in Hz. ESI-TOF spectra and HRESIMS experiments
were acquired using a Bruker maXis QTOF (Bruker Daltonik GmbH, Bremen,
Germany) mass spectrometer coupled to an Agilent 1200 LC (Agilent
Technologies, Waldbronn, Germany). Flash chromatography was performed
on a semiautomatic chromatographic system (CombiFlashTeledyne ISCO
Rf400x) with a precast reverse-phase column. Semipreparative HPLC
separation was performed on a Gilson GX-281 322H2 (Gilson Technologies,
USA) coupled to a DAD detector and an automatic fraction collector
with a semipreparative reversed-phase column (Zorbax SB-C18, 250 ×
9.4 mm, 5 μm).
on a Thermo Fisher Scientific Genesys 10S. Infrared (IR) spectra were
taken on film in a KBr window on a Perkin Elmer 500 series FTIR Panagon
1000. 1D and 2D NMR spectra were recorded on a Bruker AVANCE III spectrometer
at 500/125 MHz (1H/13C NMR, respectively) equipped
with a 1.7 mm TCI MicroCryoProbe (Bruker Biospin, Fällanden,
Switzerland). All shifts are given in δ (ppm) using the signal
of tetramethylsilane as reference. All coupling constants (J) are given in Hz. ESI-TOF spectra and HRESIMS experiments
were acquired using a Bruker maXis QTOF (Bruker Daltonik GmbH, Bremen,
Germany) mass spectrometer coupled to an Agilent 1200 LC (Agilent
Technologies, Waldbronn, Germany). Flash chromatography was performed
on a semiautomatic chromatographic system (CombiFlashTeledyne ISCO
Rf400x) with a precast reverse-phase column. Semipreparative HPLC
separation was performed on a Gilson GX-281 322H2 (Gilson Technologies,
USA) coupled to a DAD detector and an automatic fraction collector
with a semipreparative reversed-phase column (Zorbax SB-C18, 250 ×
9.4 mm, 5 μm).
3
Characterization of Organic Compounds using HPLC-MS and NMR
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Solvents employed were all HPLC grade. LRMS analyses were performed on an Agilent 1260 Infinity II (Agilent Technologies, Santa Clara, CA, USA) single quadrupole LC-MS system. HRESIMS and MS/MS spectra were acquired using a Bruker maXis QTOF mass spectrometer (Bruker Daltonik GmbH, Bremen, Germany) coupled to an Agilent 1200 Rapid Resolution HPLC. Medium pressure liquid chromatography (MPLC) was performed on a CombiFlash Teledyne ISCO Rf400x apparatus (Teledyne ISCO, Lincoln, NE, USA). Preparative or semi-preparative HPLC purifications were performed on a Gilson GX-281 322H2 HPLC (Gilson Technologies, Middleton, WI, USA). NMR spectra were recorded at 297 K on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Fällanden, Switzerland). 1H and 13C chemical shifts were reported in ppm using the signals of the residual solvents as internal reference (δH 7.26 and δC 77.0 ppm for CDCl3).
4
Analytical and Spectroscopic Characterization of Compounds
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Analytical and semipreparative HPLC analyses were conducted using a Waters Alliance (Waters Corporation, Milford, MA, USA) chromatographic system with a SunFire C18 column (10 µm, 10 × 250 mm, Waters). For UPLC analysis an Acquity UPLC equipment with a BEH C18 column (1.7 μm, 2.1 × 100 mm, Waters) was used. Optical rotations were measured using a Jasco P-2000 polarimeter (JASCO Corporation, Tokyo, Japan). UV spectra were obtained with an Agilent 1100 DAD (Agilent Technologies, Santa Clara, CA, USA). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer (JASCO Corporation, Tokyo, Japan) equipped with a PIKE MIRacleTM single reflection ATR accessory (PIKE Technologies Inc., Madison, WI, USA). NMR spectra were recorded on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Falländen, Switzerland), using the signal of the residual solvent as internal reference (δH 3.31 and δC 49.0 ppm for CD3OD). HRESIMS spectra were acquired using a Bruker maXis QTOF spectrometer (Bruker Daltonik GmbH, Bremen, Germany).
5
Comprehensive Spectroscopic Characterization
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Optical rotations were measured using a Jasco P-2000 polarimeter (JASCO Corporation, Tokyo, Japan). UV spectra were obtained with an Agilent 1100 DAD (Agilent Technologies, Santa Clara, CA, USA). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer (JASCO Corporation, Tokyo, Japan) equipped with a PIKE MIRacleTM single reflection ATR accessory (PIKE Technologies Inc., Madison, WI, USA). NMR spectra were recorded on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Falländen, Switzerland). Chemical shifts were reported in ppm using the signals of the residual solvent as internal reference (δH 7.26 and δC 77.0 for CDCl3). LC–MS and LC–HRMS analyses were performed as described previously [16 (link)].
6
Spectroscopic Characterization of Compounds
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Semipreparative HPLC was performed with an Alliance chromatographic system (Waters Corporation, Mildford, MA, USA) and an Atlantis C18 column (10 μm, 10 × 150 mm, Waters). For UPLC analysis an Acquity UPLC equipment (Waters) with a BEH C18 column (1.7 μm, 2.1 × 100 mm, Waters) was used. Optical rotations were determined with a JASCO P-2000 polarimeter (JASCO Corporation, Tokyo, Japan). IR spectrum was measured with a JASCO Fourier transform infrared (FT/IR)-4100 spectrometer (JASCO Corporation) equipped with a PIKE MIRacleTM single reflection ATR accessory. NMR spectra were recorded on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Fällanden, Switzerland), using the signal of the residual solvent as internal reference (δH 2.50 and δC 39.5 ppm for DMSO-d6). ESI-TOF MS spectra were acquired with a Bruker maXis QTOF spectrometer (Bruker Daltonik GmbH, Bremen, Germany).
7
Spectroscopic Characterization of Compounds
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Optical rotations were measured using a Jasco P-2000 polarimeter (JASCO Corporation, Tokyo, Japan). UV spectra were obtained with an Agilent 1100 DAD (Agilent Technologies, Santa Clara, CA, USA). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer (JASCO Corporation, Tokyo, Japan) equipped with a PIKE MIRacleTM single reflection ATR accessory (PIKE Thecnologies Inc., Madison, WI, USA). NMR spectra were recorded on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Falländen, Switzerland). Chemical shifts were reported in ppm while using the signals of the residual solvent as internal reference (δH 2.50 and δC 39.5 for DMSO-d6). LC–MS and LC–HRMS analyses were performed, as described previously [24 (link)].
8
Characterization of Chemical Compounds
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Optical rotations were measured using a Jasco P-2000 polarimeter (JASCO Corporation, Tokyo, Japan). UV spectra were obtained with an Agilent 1100 DAD (Agilent Technologies, Santa Clara, CA, USA). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer (JASCO Corporation, Tokyo, Japan) equipped with a PIKE MIRacleTM single-reflection ATR accessory. NMR spectra were recorded on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Falländen, Switzerland). Chemical shifts were reported in ppm using the signals of the residual solvent as internal reference (δH 2.50 and δC 39.51 for DMSO-d6). LC-MS and LC-HRMS analyses were performed as described previously [26 (link)].
9
Spectroscopic Characterization of Compounds
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Optical rotations were measured using a Jasco P-2000 polarimeter (JASCO Corporation, Tokyo, Japan). UV spectra were obtained with an Agilent 1100 DAD (Agilent Technologies, Santa Clara, CA, USA). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer (JASCO Corporation, Tokyo, Japan) equipped with a PIKE MIRacleTM single reflection ATR accessory (PIKE Thecnologies Inc., Madison, WI, USA). NMR spectra were recorded on a Bruker Avance III spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) equipped with a 1.7 mm TCI MicroCryoProbeTM (Bruker Biospin, Falländen, Switzerland). Chemical shifts were reported in ppm using the signals of the residual solvent as internal reference (δH 3.31 and δC 49.15 for CD3OD). LC–MS and LC–HRMS analyses were performed as described previously [23 (link)].
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