Mercury vxr 300 spectrometer

The mass spectra were recorded on GCMS-Q1000-EX Shimadzu and GCMS 5988-A HP spectrometers, and the ionizing voltage was 70 eV (Tokyo, Japan). The IR spectra were recorded in potassium bromide discs on Shimadzu FT IR 8101 PC infrared spectrophotometer (Shimadzu, Tokyo, Japan). The ¹H- and ¹³C-NMR spectra were recorded on Varian Mercury VXR-300 spectrometer (300 MHz for ¹H-NMR and 75 MHz for ¹³C-NMR), and the chemical shifts were related to those of the solvent DMSO-d₆ (Varian, Inc., Karlsruhe, Germany). All reactions were followed by thin-layer chromatography (TLC) (silica gel, Aluminum Sheets 60 F254, Merck, Cairo, Egypt). Elemental analyses were carried out at the Microanalytical Centre of Cairo University, Giza, Egypt. Sonication was performed in Shanghai Branson-CQX ultrasonic cleaner at a frequency of 40 kHz, and ultrasonic power was kept at 250 W.

All of the corrected melting points are in degree centigrade and measured using a Stuart SMP20 melting point apparatus (Bibby Scientific Limited, Staffordshire, UK). The infrared spectra were recorded on a PerkinElmer Alpha platinum-ATR spectrometer; the ¹H-NMR (300 MHz) and ¹³C-NMR (75 MHz) spectra were recorded on a Varian Mercury VXR-300 spectrometer (Varian Inc., Palo Alto, CA, USA) and the chemical shifts were related to that of the solvent DMSO-d₆ using tetramethylsilane (TMS) as an internal standard. MS spectra (HRMS) were acquired on TRACE GC Ultra gas chromatograph mass spectrometry, coupled with a THERMO mass spectrometer detector ISQ Single Quadrupole Mass Spectrometer (THERMO Scientific Corp., Waltham, MA, USA)and were obtained by electron ionization (EI) at 70 eV, using a spectral range of m/z 50–1000.All of the microanalyses and spectral analyses were performed by the Micro Analytical Centers of Taif University-Saudi Arabia (IR spectra, HRMS), Cairo University (¹H-NMR, ¹³C-NMR), and National Research Center-Egypt (Mass spectra).

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.