5988 spectrometer

All melting points (°C) were recorded using a Fisher–John melting point apparatus and were uncorrected. The IR spectra were determined for KBr discs on a Thermo Fischer Scientific Nicolet IS10 spectrometer (wavenumber in cm⁻¹) at the Faculty of Pharmacy, Mansoura University, Egypt. The ¹H NMR spectra were obtained in DMSO-d₆ or CDCl₃ employing a Jeol 500 MHz spectrometer at the Faculty of Science, Mansoura University, Egypt. The ¹³C NMR spectra were obtained in DMSO-d₆ using a Jeol 500 MHz spectrometer at the Faculty of Science, Mansoura University, Egypt. Electron ionisation mass spectrometry (EI MS) was performed on a Hewlett Packard 5988 spectrometer at the Al-Azhar University, Cairo, Egypt. Microanalyses (C, H, N) were conducted at the Microanalytical Unit, Cairo University, and the results were within ±0.4% of the theoretical values. The antiproliferative screening of all newly synthesised compounds, enzyme activity inhibition assay, caspase-3 assay, apoptosis induction analysis, and cell cycle analysis was conducted at the Holding Company for Biological Products and Vaccines (VACSERA), Cairo, Egypt.

Melting points were determined using a Griffin apparatus and were uncorrected. IR spectra were recorded on a Shimadzu IR-435 spectrophotometer using KBr discs and values were represented in cm⁻¹. ¹H NMR and ¹³C NMR (DEPT-Q) were carried out on Bruker apparatus at 400 MHz for ¹H NMR and 100 MHz for ¹³C NMR spectrophotometer, (Faculty of Pharmacy, Beni-Suef University, Beni-Suef, Egypt), in DMSO-d₆, D₂O using TMS as an internal standard and chemical shifts were recorded in ppm on δ scale using DMSO-d₆ (2.5) as a solvent. Coupling constant (J) values were estimated in Hertz (Hz). Splitting patterns are designated as follows: s, singlet; d, doublet, t, triplet; q, quartet; dd, doublet of doublet; m, multiplet. The electron impact (EI) mass spectra were recorded on Hewlett Packard 5988 spectrometer (Palo Alto, CA). Microanalysis was performed for C, H, N on Perkin-Elmer 2400 at the Microanalytical center, Cairo University, Egypt and was within ±0.4% of theoretical values. Analytical thin-layer chromatography (TLC): pre-coated plastic sheets, 0.2 mm silica gel with UV indicator (Macherey-Nagel) was employed routinely to follow the course of reactions and to check the purity of products. All other reagents, solvents and compound 1 were purchased from the Aldrich Chemical Company (Milwaukee, WI), were used without further purification.

Melting points were determined using the Griffin apparatus and were uncorrected. Values of IR spectra were measured using Shimadzu IR-435 spectrophotometer with KBr discs and represented in cm⁻¹. ¹H NMR and ¹³C NMR were carried out using the Bruker instrument at 400 MHz for ¹H NMR and 100 MHz for ¹³C NMR spectrophotometer, (Faculty of Pharmacy, Beni-Suef University, Beni-Suef, Egypt), in DMSO-d6 (as a solvent), D₂O using TMS as an internal standard and chemical shifts were recorded in ppm on the δ scale using DMSO-d6 (2.5) as a solvent. Coupling constant (J) values were estimated at Hertz (Hz). Splitting patterns were designated as follows: s, singlet; d, doublet, t, triplet; q, quartette; m, multiplet. Hewlett Packard 5988 spectrometer (Palo Alto, CA) was used to record the electron impact (EI) mass spectra (Microanalytical centre, Cairo University). Microanalysis was performed for C, H, and N on Perkin-Elmer 2400 at the Microanalytical Centre, Cairo University, Egypt and was within ±0.4% of theoretical values. Analytical thin-layer chromatography (TLC), pre-coated plastic sheets, 0.2 mm silica gel with UV indicator (Macherey-Nagel) was employed routinely to follow the course of reactions and to check the purity of products. All other reagents, solvents and compound 1 were purchased from the Aldrich Chemical Company (Milwaukee, WI) and were used without further purification.