All reagents and solvents were obtained from commercial suppliers and used without further purification. The reactions were monitored by thin layer chromatography (TLC), using MERCK pre-coated silica gel 60-F254 aluminum plates. Column chromatography with 60–120 mesh silica gel was used as separation and purification method. Ethyl acetate and hexane were used as eluents. Melting points were obtained on Stuart digital melting-point apparatus/SMP 30 and were uncorrected. All IR spectra were recorded on a Perkin Elmer, FT-IR spectrometer using KBr discs. 1H NMR spectra were recorded on an Avance NMR instrument operated at 500 MHz. 13C NMR spectra were recorded on an Avance NMR instrument operated at 125 MHz. Chemical shift values were reported in ppm with TMS as an internal reference and J values were given in Hertz. The following abbreviations were used for 1H NMR spectra to indicate the signal multiplicity: s (singlet), d (doublet), dd (doublet of doublet), and m (multiplet). HRMS were determined with Agilent QTOF mass spectrometer 6540 series instrument using ESI technique.
Qtof mass spectrometer 6540 series instrument
Manufactured by Agilent Technologies
The Agilent 6540 series QTOF mass spectrometer is a high-resolution, accurate-mass instrument designed for analytical applications. It features a quadrupole time-of-flight (QTOF) configuration, which provides precise mass measurements and detailed structural information about analyzed compounds.
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5 protocols using qtof mass spectrometer 6540 series instrument
1
Synthesis and Characterization of Novel Compounds
2
Synthetic Procedures and Characterization
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Materials and methods : All the reagents and solvents were obtained from commercial suppliers and were used without further purification. Analytical thin-layer chromatography (TLC) was performed on MERCK precoated silica gel 60-F254 (0.5 mm) aluminium plates. Visualization of the spots on TLC plates was achieved by UV light. Wherever required, column chromatography was performed using silica gel (60–120). The reactions wherever anhydrous conditions are required were carried under nitrogen positive pressure using freshly distilled solvents. All evaporation of solvents was carried out under reduced pressure using a rotary evaporator below 45 °C. 1H and 13C NMR spectra were recorded on Bruker 500 MHz by making a solution of samples in the DMSO using tetramethylsilane (TMS) as the internal standard. Chemical shifts for 1H and 13C are reported in parts per million (ppm) downfield from tetramethylsilane. Spin multiplicities are described as s (singlet), d (doublet), t (triplet), q (quartet), and m (multiplet). Coupling constant (J) values are reported in hertz (Hz). HRMS was determined with Agilent QTOF mass spectrometer 6540 series instrument. Melting points were determined with an electrothermal digital melting point apparatus IA9100 and are uncorrected. The names of all the compounds given in the experimental section were taken from Chem Bio Draw Ultra, Version 12.0.
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3
Synthesis and Characterization of Novel Organic Compounds
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All the commercially available reagents were used without further purification. Solvents were dried and distilled wherever necessary prior to use using standard methods. All the air and moisture sensitive reactions were performed under inert conditions using clean and dried glassware and syringe technique to transfer solutions. Reactions were monitored by TLC using Merck silica gel 60 F-254 plates. Purification was performed by column chromatography on silica gel (60–120 mesh) using a mixture of DCM and methanol as eluent. Melting points were acquired on Stuart digital melting point apparatus/SMP 30 in open capillary tubes and uncorrected. Nuclear Magnetic Resonance (1H NMR and 13C NMR) spectra were recorded by using an Avance bruker 500 and 125 MHz spectrometer in DMSO-d6 as solvent and tetramethylsilane as internal standard. Chemical shifts are reported as δ values in parts per million (ppm) and coupling constants (J) are expressed in Hz. Multiplicities are described as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), dd (doublet of doublets). HRMS were determined with Agilent QTOF mass spectrometer 6540 series instrument and were performed in the ESI techniques at 70 eV.
4
Synthesis and Characterization of Organic Compounds
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All solvents were purified and dried using standard methods prior to use. Commercially available reagents were used without further purification. All reactions involving air- or moisture-sensitive compounds were performed under a nitrogen atmosphere using dried glassware and syringe techniques to transfer solutions. Analytical thin-layer chromatography (TLC) was carried out on Merck silica gel 60 F-254 aluminium plates. Melting points were determined on Stuart digital melting-point apparatus/SMP 30 in open capillary tubes and uncorrected. Nuclear magnetic resonance (1H-NMR, 13 C-NMR) spectra were recorded using an Avance Bruker 500 MHz, 125 MHz spectrometer in DMSO-d6. Chemical shifts reported in parts per million (ppm) with TMS as an internal reference, and the coupling constants (J) expressed in hertz (Hz). Splitting patterns are denoted as follows: s, singlet; d, doublet; t, triplet; m, multiplet; dd, doublet of doublet. HRMS were determined with Agilent QTOF mass spectrometer 6540 series instrument and were performed in the ESI techniques at 70 eV.
5
Synthesis and Characterization of Target Compounds
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The target compounds were synthesized from commercially available reagents without further purification. The solvents were distilled and dried following standard methods as necessary prior to their use. All the air and moisture sensitive reactions were kept under inert conditions using clean and dried glassware and a syringe technique to transfer the solutions. The reactions were monitored via thin layer chromatography (TLC) using Merck silica gel 60F–254 plates. The synthesized molecules were purified by washing them with a mixture of 5–10% ethylacetate in hexane. The melting points were acquired using Stuart digital melting point apparatus (SMP 30) in open capillary tubes, and they were uncorrected. Nuclear Magnetic Resonance (1H NMR and 13C NMR) spectra were recorded using an Avance Bruker 500 MHz and 125 MHz spectrometer in DMSO-d6 as the solvent and tetramethylsilane (TMS) as the internal standard. Chemical shifts were represented as δ values in parts per million (ppm) and coupling constants (J) in Hz. Multiplicities were described as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), and dd (doublet of doublets). HRMS were determined using the Agilent QTOF mass spectrometer 6540 series instrument, and they were performed via ESI techniques at 70 eV.
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