Jms 600 mass spectrometer

All reagents, chemicals and solvents of analytical grade were purchased from Sigma-Aldrich Co. USA. The TLC plates were purchased from the local market. All other chemicals were of analytical grade and were used without further purification. Melting points were determined on an Electrothermal 9100 melting point apparatus (Weiss-Gallenkamp, Loughborough, UK). Compounds purity were confirmed by Thin Layer Chromatography (TLC) using Kieselgel 60 F254 (Merck). EI-MS was performed on JEOL JMS 600 mass spectrometer. We have performed Elemental analyses of all synthesized compounds with an Elementar-Vario EL instrument. ¹H-NMR Bruker signals appeared at 600 MHz in CH₃OH-d⁴ and that of ¹³C-NMR at 150 MHz in CHCl₃-d.^{4 (link)}

Melting points are uncorrected.
The IR spectra were recorded on a Shimadzu 440 infrared spectrophotometer
(υ/cm^–1) using the KBr technique (Shimadzu,
Japan). ¹H NMR spectra were recorded on a Varian Gemini
spectrometer (δ/ppm) 300 and 400 MHz using TMS as an internal
standard. Mass spectra were recorded on a Jeol-JMS-600 mass spectrometer. ¹³C NMR spectra were run at 75 and 101 MHz. Micro analytical
data were obtained from the Micro Analytical Research Centre, Faculty
of Science, Cairo University. The reactions were monitored by thin
layer chromatography (TLC) using TLC sheets with UV fluorescent silica
gel Merck 60f254 plates using a UV lamp and different solvents as
mobile phases. 2-(4-Oxothiazolidin-2-ylidene)acetonitrile (1a) and ethyl-2-(4-oxothiazolidin-2-ylidene)acetate (1b) were prepared according to the reported method.^{35 (link)} Furthermore, 1,3-diphenyl-1H-pyrazole-4-carbaldehyde
(2a), 1-phenyl-3-(p-tolyl)-1H-pyrazole-4-carbaldehyde (2b),^{37 (link)} 2-cyano-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)acetamide (9),^{41 (link),56 (link)} and N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)carbonohydrazonoyldicyanide (12)^{42 (link)} were also prepared.