Pure samples were measured separately as MeOH solutions and various diagnostic shift reagents, Shimadzu ultraviolet (UV) 240 spectrophotometer,[19 ] and with sprayed Naturstoff reagent.[20 ] Nuclear magnetic resonance (NMR) analyses were run on Varian Mercury 300 MHz and Bruker 500 MHz spectrometers relative to TMS in different deuterated solvents. Electrospray ionization-mass spectrometry (ESI-MS) spectra were measured according to previously published conditions.[18 ]
Mercury 300 mhz
Manufactured by Bruker
Sourced in United Kingdom
The Mercury 300 MHz is a nuclear magnetic resonance (NMR) spectrometer designed for routine analysis and structural characterization of samples. It offers a magnetic field strength of 300 MHz and is capable of performing high-resolution 1D and 2D NMR experiments. The core function of the Mercury 300 MHz is to provide accurate and reliable NMR data for various applications.
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Lab products found in correlation
343 polarimeter, by PerkinElmer (2 mentions)
Lcq fleet spectrometer, by Thermo Fisher Scientific (2 mentions)
Avance 1 400 mhz spectrometers, by Bruker (2 mentions)
Q tof microspectrometer, by Waters Corporation (1 mentions)
Masslynx software, by Waters Corporation (1 mentions)
Avance 400 mhz, by Bruker (1 mentions)
681 spectrometer, by PerkinElmer (1 mentions)
Agilent 1100 lc msd trap system vl, by Agilent Technologies (1 mentions)
5 protocols using mercury 300 mhz
1
Detailed Spectroscopic Analysis of Samples
2
NMR and Mass Spectroscopic Characterization
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NMR spectroscopic experiments were carried out, either on Varian MERCURY 300 MHz (300 and 75 MHz for 1H and 13C, respectively) or Bruker Avance I 400 MHz spectrometers (400 and 101 MHz for 1H and 13C, respectively). Chemical shifts (δ) are given in ppm relative to the CHCl3 internal standard, and the coupling constants J are reported in Hertz (Hz). Mass spectra were recorded on an LCQESI MS, on a LCQ Advantage spectrometer from Thermo Finningan, and a LCQ Fleet spectrometer from Thermo Scientific. Optical rotations were measured on a PerkinElmer 343 polarimeter (concentration in g/100 mL). Diazoalkanes 1a –c , maleimides 2a,b, and protected amino acids are commercially available compounds.
3
NMR, MS, and Optical Rotation Analysis
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NMR spectroscopic experiments were
carried out either on Varian MERCURY 300 MHz (300 and 75 MHz for 1H and 13C, respectively) or Bruker Avance I 400
MHz spectrometers (400 and 101 MHz for 1H and 13C, respectively). Chemical shifts (δ) are given in ppm relative
to the CHCl3 internal standard, and the coupling constants J are reported in Hertz (Hz). Mass spectra were recorded
on an LCQESI MS and on a LCQ Advantage spectrometer from Thermo Finningan
and a LCQ Fleet spectrometer from Thermo Scientific. Optical rotations
were measured on a PerkinElmer 343 polarimeter (concentration in g/100
mL). Diazoalkanes1a –c and maleimides 2a –c are commercially available compounds.
carried out either on Varian MERCURY 300 MHz (300 and 75 MHz for 1H and 13C, respectively) or Bruker Avance I 400
MHz spectrometers (400 and 101 MHz for 1H and 13C, respectively). Chemical shifts (δ) are given in ppm relative
to the CHCl3 internal standard, and the coupling constants J are reported in Hertz (Hz). Mass spectra were recorded
on an LCQESI MS and on a LCQ Advantage spectrometer from Thermo Finningan
and a LCQ Fleet spectrometer from Thermo Scientific. Optical rotations
were measured on a PerkinElmer 343 polarimeter (concentration in g/100
mL). Diazoalkanes
4
NMR and MS Spectral Analysis
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NMR spectra were recorded on Varian Mercury 300 MHz and/or on Bruker Avance 400 MHz instrument using CD 3 OD or D 2 O as deuterated solvents; the chemical shift was expressed in ppm from TMS.
MS spectra were performed on a Q-TOF MICRO spectrometer (Micromass, now Waters, Manchester, UK) equipped with an ESI source, that operated in the negative and/or positive ion mode. The flow rate of sample infusion was 10 lL/min with 100 acquisitions per spectrum. Data were analyzed by using the MassLynx software developed by Waters.
Solvents of RPE grade were purchased from Sigma Aldrich or Carlo Erba Reagenti, silica gel 60 (70-230 mesh ASTM) from Fluka.
MS spectra were performed on a Q-TOF MICRO spectrometer (Micromass, now Waters, Manchester, UK) equipped with an ESI source, that operated in the negative and/or positive ion mode. The flow rate of sample infusion was 10 lL/min with 100 acquisitions per spectrum. Data were analyzed by using the MassLynx software developed by Waters.
Solvents of RPE grade were purchased from Sigma Aldrich or Carlo Erba Reagenti, silica gel 60 (70-230 mesh ASTM) from Fluka.
5
Spectroscopic Characterization of Synthesized Compounds
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Melting points taken on an Electrothermal apparatus were uncorrected.
1 H NMR and 13 C NMR spectra were recorded on a Varian-Mercury 300 MHz, Bruker-Aspect 3000 console 500 MHz spectrometer, or Bruker 600 MHz; chemical shifts are reported in parts per million (d). FT-IR spectra were recorded on a Perkin-Elmer 681 spectrometer. Thin-layer chromatography (TLC) was performed on silica gel sheets with fluorescent indicator. The spots on the TLC were visualized under ultraviolet light. Chromatography was conducted by using silica gel 60 with a particle size distribu tion of 40e63 mm and 230e400 ASTM. MS-ESI analyses were performed on Agilent 1100 LC/MSD trap system VL. All synthesized compounds were analyzed by CHN or by HPLC analysis performed on an Agilent 1260 Infinity instrument equipped with a 1260 DAD VLþ detector, and their purity is higher than 95%.
1 H NMR and 13 C NMR spectra were recorded on a Varian-Mercury 300 MHz, Bruker-Aspect 3000 console 500 MHz spectrometer, or Bruker 600 MHz; chemical shifts are reported in parts per million (d). FT-IR spectra were recorded on a Perkin-Elmer 681 spectrometer. Thin-layer chromatography (TLC) was performed on silica gel sheets with fluorescent indicator. The spots on the TLC were visualized under ultraviolet light. Chromatography was conducted by using silica gel 60 with a particle size distribu tion of 40e63 mm and 230e400 ASTM. MS-ESI analyses were performed on Agilent 1100 LC/MSD trap system VL. All synthesized compounds were analyzed by CHN or by HPLC analysis performed on an Agilent 1260 Infinity instrument equipped with a 1260 DAD VLþ detector, and their purity is higher than 95%.
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