All the chemicals and solvents were procured and utilised as such from the suppliers. Wherever necessary, anhydrous solvents were used. Thin layer chromatography (TLC) analysis was done by utilising Merck silica gel 60 F254 aluminium plates. Stuart digital melting point apparatus (SMP 30) was used in determining the melting points of the compounds, which are uncorrected. 1H and 13C NMR spectra were recorded using Bruker Avance 500 MHz and 125 MHz respectively using DMSO-d6 as the solvent. Chemical shift values are recorded in ppm using TMS as the internal standard. HRMS were determined by Agilent QTOF mass spectrometer 6540 series instrument and were performed using ESI techniques at 70 eV.
Qtof mass spectrometer 6540 series
Manufactured by Agilent Technologies
The Agilent 6540 series QTOF mass spectrometer is a high-resolution, accurate-mass instrument designed for advanced analytical applications. It utilizes quadrupole time-of-flight (QTOF) technology to provide accurate mass measurements and high-resolution data. The instrument is capable of performing both full-scan and targeted MS/MS analysis.
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Lab products found in correlation
3 protocols using qtof mass spectrometer 6540 series
1
Spectroscopic Analysis of Organic Compounds
2
Facile Synthesis of Fluorinated Compounds
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All the chemicals, reagents and starting materials were procured from commercial providers and were used as such. The monitoring of reactions was performed by TLC-MERCK pre-coated silica gel 60-F254 (0.5 mm) aluminium plates under UV light. 1H and 13C NMR spectra were obtained on Bruker Avance 500 MHz spectrometer using tetramethyl silane (TMS) as the internal standard and chemical shifts are reported in ppm. Chemical shifts are referenced to TMS (δ 0.00 for 1H NMR and 13C NMR) and corresponding solvents used for NMR recording CDCl3 (δ 7.26 for 1H NMR and 77.2 13C NMR) or DMSO/d6 (δ 2.50 for 1H NMR and 39.5 for 13C NMR). Spin multiplicities for 1H NMR are reported as s (singlet), brs (broad singlet), d (doublet), dd (double doublet), t (triplet) and m (multiplet). Unless and otherwise mentioned, values in 13C NMR are implicated as single Carbon while multiple Carbon is shown as ‘nC’ where n implies no. of Carbon. Coupling constant (J) values are reported in hertz (Hz). In 13C NMR of Fluorine containing compound, Carbon–Fluorine coupling is denoted by JCF. HRMS were determined with Agilent QTOF mass spectrometer 6540 series instrument and were performed in the ESI techniques at 70 eV. Column chromatography was performed using silica gel 60–120 or 100–200 mesh. Melting point was taken using Stuart® SMP30 apparatus.
3
Optimization of Silica Gel Purification
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Unless otherwise specified, all solvents and other reagents are commercially available and used without further purification. All reagents were weighed and handled in air at room temperature. Column chromatography was performed on silica gel (60–120 and 100–200 mesh). NMR spectra were recorded on Bruker 500 NMR spectrometer. Chemical shifts were mentioned in parts per million (ppm, δ). Proton coupling patterns are described as singlet (s), doublet (d), triplet (t), quartet (q), doublet of doublet (dd), doublet triplet (dt) and multipet (m). HRMS were determined in negative mode with Agilent QTOF mass spectrometer 6540 series instrument. Melting points are determined on an electro thermal melting point apparatus and are uncorrected. The names of all compounds given in the Experimental section were taken from Chem ultra, version 12.0. The reactions wherever anhydrous conditions required are carried under nitrogen positive pressure using freshly distilled solvents. All evaporation of solvents was carried out under reduced pressure on Heidolph rotary evaporator below 40–45 °C.
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