Avance av 400 mhz spectrometer

Analytical grade reagents and solvents for synthesis and analysis which included m-toluic acid and o-phenylenediamine were obtained from Sigma Aldrich (USA) whilst pyridine, thionyl chloride, hexane, methanol, ethyl acetate and dimethyl sulfoxide were obtained from Merck Chemicals (SA). The chemicals were used as received (i.e. without further purification). 1 H NMR and 13 C NMR spectra were recorded on a Bruker Avance AV 400 MHz spectrometer operating at 400 MHz for 1 H and 100 MHz for 13 C using DMSO-d 6 as solvent and tetramethylsilane as internal standard. Chemical shifts are expressed in ppm. FT-IR spectra were recorded on a Bruker platinum ATR spectrophotometer Tensor 27. Elemental analyses were performed using a Vario Elementar Microcube ELIII. Melting points were obtained using a Stuart Lasec SMP30 whilst the masses were determined using Agilent 7890A GC System connected to a 5975C VL-MSC with electron impact as the ionization mode and a triple-axis detector. The GC was fitted with a 30 m × 0.25 mm × 0.25 μm DB-5 capillary column. Helium was used as carrier gas at a flow rate of 1.63 mL/min with an average velocity of 30.2 cm/s and a pressure of 63.7 kPa.