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Part-IExperimental4. ExperimentalAll the chemicals used in the synthesis were of laboratory grade. The melting points weredetermined in open capillary method on Veego (VMP-D) electronic apparatus and areuncorrected.The IR spectra of synthesized compounds were recorded on Shimadzu 8400-S FT-IR, aswell as, Perkin Elmer BX 2 FT-IR Spectrophotometer in potassium bromide discs.1 H NMR spectra were recorded on a Bruker AC 400 MHz FT-NMR spectrometer usingTMS (Tetramethyl silane) as an internal standard and DMSO-d 6 as a solvent at SAIF,Punjab <strong>University</strong>, Chandigarh.Mass spectra were obtained by Electron Impact method on (GCMS-QP2010spectrometer) using 70 eV ionizing beam and using direct insertion probe.To monitor the reactions, as well as, to establish the identity and purity of reactants andproducts, thin layer chromatography was performed on precoated silica plates (MerckSilicagel F 254 ) using hexane-ethyl acetate-glacial acetic acid as the solvent systems andthe spots were visualized by exposure to iodine vapors or under ultra violet (UV) light at254 nm and 360 nm.4.1 Synthesis of Starting Materials4.1.1 Synthesis of chloroacetonitrile (CAS # 107142) 1,2 :a. Synthesis of chloroacetamideIn a 2 liter round-bottomed flask, fitted with a mechanical stirrer and surrounded by anice-bath was placed 215 gm (1.75 mole) of ethyl chloroacetate. To the vigorously stirredcold ester, 200 ml of chilled aq. ammonia (sp. gr 0.9) was added. The solution was stirredin the cold for further 30 min; thereafter another 200 ml portion of aq. ammonia wasadded and the stirring was continued for about 15 min. The mixture was then allowed tostand for 30 min at 0-5 o C, filtered under suction and washed with 25 ml portion of coldwater to remove ammonium chloride. The yield of air-dried material, melting at 118-165

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