Gcms 5988 a hp spectrometers

Melting points were measured on an electrothermal Gallenkamp capillary apparatus (Leicester, UK) and are uncorrected. Elemental analyses were carried out at the Microanalytical Center of Cairo University, Giza, Egypt. The IR spectra were recorded on a Pye-Unicam SP300 Instrument (Cambridge, UK) in potassium bromide discs. The ¹H NMR (nuclear magnetic resonance) and ¹³C NMR of the newly synthesized compounds in DMSO-d₆ were measured on a Varian Mercury VXR-300 spectrometer (Varian, Karlsruhe, Germany) at 300 MHz for ¹H NMR and 75 MHz for ¹³C NMR) and the chemical shifts were related to that of the solvent. The mass spectra were recorded on a GCMSQ1000-EX Shimadzu (Tokyo, Japan) and GCMS 5988-A HP spectrometers (Shimadzu, Tokyo, Japan) where the ionizing voltage was 70 eV. Microwave experiments were carried out using CEM Discover Labmate microwave apparatus (Discover, SP, NC, USA, 300 W). The starting materials 2-{1-[4-((4-methylphenyl)sulfonamide) phenyl]ethylidine}thiosemicarbazide 1 [14 (link)], α-keto hydrazonoyl halides 2a–j [15 (link),16 (link),17 (link),18 (link)], and arenecarbohydrazonoyl halides 5a–d [19 (link),20 (link)] were prepared as reported in literature.

Melting points of crystalline azo compounds were measured on an electrothermal Gallenkamp apparatus and are not corrected. Solvents were generally distilled and dried by standard literature procedure prior to use. The UV-Vis spectra were recorded on a Perkin-Elmer Lambada 40 spectrometer (Perkin-Elmer, Überlingen, Germany). The IR spectra were taken with a Pye-Unicam SP300 spectrometer using KBr discs (Shimadzu, Tokyo, Japan) The ¹H NMR (300 MHz) spectra were obtained with a Varian Mercury VXR-300 spectrometer (Varian, Inc., Karlsruhe, Germany). Mass spectra were recorded on a GC-MS Q1000-EX (Shimadzu, Tokyo, Japan) and GC-MS 5988-A HP spectrometers (Shimadzu, Tokyo, Japan), the ionizing voltage was 70 eV. Elemental analyses were carried out by the Micro analytical Center of Cairo University, Giza, Egypt. 5-arylazosalicylaldehyde 4a [29 ] and 4b,c,g,i [30 ] were prepared by literature methods and 1-methyl-4-(2-hydroxystryl)pyridinium iodide 7 [31 (link)]. Typical reaction procedures and spectroscopic data for the all new products are listed below.