Chn analyzer model

Melting points (Mps) were determined with a Kofler hot-stage apparatus and were uncorrected. Elemental analyses were performed with a Perkin-Elmer CHN analyzer model. Thin-layer chromatography was performed on silica gel 60 F254 (layer thickness 0.2 mm, Merck, Rahway, NJ, USA); eluents: (A) 70% ethyl acetate/30% hexane, (B) 30% ethyl acetate/70% hexane. The spots were detected with I₂ or UV (365 nm) after spraying with 5% phosphomolybdic acid in 50% aqueous phosphoric acid and heating at 100–120 °C for 10 min. Flash chromatography was performed on silica gel 60, 40–63 μm (Merck). ¹H NMR spectra were recorded in DMSO-d₆ or CDCl₃ solution with a Bruker DRX-500 instrument at 500 MHz. ¹³C NMR spectra were recorded with the same instrument at 125 MHz under the same conditions. Mass spectrometry: Full-scan mass spectra of the newly synthesized compounds were acquired in the range of 100 to 1100 m/z with a Q Exactive Plus quadrupole-orbitrap mass spectrometer (Thermo Fisher Scientific, Waltham, MA, USA) equipped with a heated electrospray (HESI). Analyses were performed in positive ion mode using flow-injection mass spectrometry with a mobile phase of 50% aqueous acetonitrile containing 0.1 v/v% formic acid (0.3 mL/min flow rate). Aliquots of 5 µL of samples were injected into the flow. The ESI capillary was adjusted to 3.5 kV, and N₂ was used as a nebulizer gas.

Thin-layer chromatography (TLC) was employed to track all reactions utilizing percolated dishes of silica gel G/UV-254 with a 0.25 mm thickness (Merck 60F254) and UV light (254 nm/365 nm) enable visualization. The uncorrected Kofeler melting point instrument was used to record all melting points. On an FT-IR spectrophotometer, KBr pellets were used to analyze IR spectra. At Sohag University, ¹H-NMR and ¹³C-NMR (DMSO-d₆) spectra were captured at 400 M Hz and 100 MHz, respectively. For ¹H-NMR data, the following information is provided: chemical shift, integration, and multiplicity (singlet, doublet, triplet, multiplet). Tetramethylsilane (TMS) was selected as the standard for internal measurement, and its chemical shifts (δ) were expressed in parts per million (ppm). TMS (= 0 ppm) or DMSO (= 39.51 ppm) was employed as internal standards for ¹³C-NMR. A Perkin-Elmer CHN analyzer model provided the elemental analyses.