13c nmr spectrophotometer

Melting points were measured on the Griffin apparatus and were uncorrected. Determination of IR spectra was achieved using Shimadzu IR-435 spectrophotometer with KBr discs and values were obtained in cm⁻¹. ¹H NMR and ¹³C NMR were recorded on Bruker instrument at 400 MHz for ¹H NMR and 100 MHz for ¹³C NMR spectrophotometer (Faculty of Pharmacy, Mansoura University, Mansoura, Egypt), in DMSO-d₆ (as a solvent), D₂O using TMS as an internal standard and chemical shifts (δ) were expressed in parts per million (ppm) compared to internal standard, TMS (δ = 0 ppm). Coupling constant (J) values were expressed in Hertz (Hz). Signal splitting patterns were designated as follows: s, singlet; d, doublet, t, triplet; q, quartette; m, multiplet. The electron impact (EI) mass spectra were carried out using Hewlett Packard 5988 spectrometer (Palo Alto, CA) at Faculty of Science, Cairo University, Giza, Egypt. Microanalysis was calculated for C, H, N on Perkin-Elmer 2400 at the Microanalytical centre, Faculty of Science, Cairo University, Egypt and was within ±0.4% of theoretical values. The progress of the reaction and purity of products were monitored by thin layer chromatography (TLC), pre-coated plastic sheets, 0.2 mm silica gel with UV indicator (Macherey-Nagel, Düren, Germany). All used reagents and solvents were purchased from the Aldrich Chemical Company (Milwaukee, WI).

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.