All reactions were carried out in oven-dried glassware under an atmosphere of dry N2 with the rigid exclusion of air and moisture using standard Schlenk techniques. Dichloromethane was freshly distilled from CaH2 immediately before use. All other chemicals were purchased from either J&K Chemical Co. or used as received unless otherwise specified. 1H and 13C{1H} NMR (Nuclear magnetic resonance) spectra were recorded on a Varian Inova 400 spectrometer at 400 and 100 MHz, respectively. All signals were reported in ppm unit with references to the residual solvent resonances of the deuterated solvents for proton and carbon chemical shifts. Mass spectra were obtained on a Thermo Finnigan MAT 95 XL spectrometer, Shanghai Institute of Organic Chemistry, CAS.
Finnigan mat95xl spectrometer
Manufactured by Thermo Fisher Scientific
The Finnigan MAT95XL is a high-performance mass spectrometer designed for a wide range of analytical applications. It features a dual-focusing magnetic-sector design and can operate in both positive and negative ion mode. The Finnigan MAT95XL is capable of performing various mass spectrometric techniques, including electron ionization, chemical ionization, and high-resolution mass analysis.
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3 protocols using finnigan mat95xl spectrometer
1
Schlenk Techniques for Organometallic Synthesis
2
Spectroscopic Characterization of Synthesized Compounds
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Melting points were determined on a Mel-Temp melting point apparatus in open capillaries and were uncorrected. Infrared (IR) spectra were recorded using 1725XFT-IR spectrophotometer. High-resolution mass spectra (HRMS) were obtained on a Thermo Fisher Scientific Finnigan MAT95XL spectrometer using a magnetic sector analyzer. Peptide mass analysis was obtained by MALDI TOF MS (Bruker), and peptide purity was confirmed by RP-HPLC (Hitachi). 1H NMR (400 MHz) and 13C NMR (100) spectra were recorded on a Bruker 400 spectrometer. Chemical shifts were reported in parts per million on the scale relative to an internal standard (tetramethylsilane, or appropriate solvent peaks) with coupling constants given in hertz. 1H NMR multiplicity data are denoted by s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet). Analytical thin-layer chromatography (TLC) was carried out on Merck silica gel 60G-254 plates (25 mm) and developed with the solvents mentioned. Visualization was accomplished by using portable UV light, and an iodine chamber. Flash chromatography was performed in columns of various diameters with Merck silica gel (230–400 mesh ASTM 9385 Kieselgel 60H) by elution with the solvent systems. Solvents, unless otherwise specified, were reagent grade and distilled once before use. All new compounds exhibited satisfactory spectroscopic and analytical data.
3
Spectroscopic Characterization of Organic Compounds
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Melting points were determined on a Mel-Temp melting point apparatus in open capillaries and are uncorrected. Infrared (IR) spectra were recorded using 1725XFT-IR spectrophotometer. High resolution mass spectra (HRMS) were obtained on a Thermo Fisher Scientific Finnigan MAT95XL spectrometer using magnetic sector analyzer. 1H NMR (400 MHz) and 13C NMR (100) spectra were recorded on a Bruker 400 spectrometer. Chemical shifts were reported in parts per million on the scale relative to an internal standard (tetramethylsilane, or appropriate solvent peaks) with coupling constants given in hertz. 1H NMR multiplicity data are denoted by s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet). Analytical thin-layer chromatography (TLC) was carried out on Merck silica gel 60G-254 plates (25 mm) and developed with the solvents mentioned. Visualization was accomplished by using portable UV light, ninhydrin spray, or iodine chamber. Flash chromatography was performed in columns of various diameters with Merck silica gel (230–400 mesh ASTM 9385 kieselgel 60H) by elution with the solvent systems. Solvents, unless otherwise specified, were reagent grade and distilled once prior to use. All new compounds exhibited satisfactory spectroscopic and analytical data.
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