preview

Zinc Sulfamate Lab Report

Decent Essays
Open Document

All reagents and intermediates were obtained from commercial suppliers and used without any further purification. Zinc oxide (99.0%), sulphamic acid (99.0%), acetonitrile (HPLC grade), ethyl acetate (98.0%), anhydrous sodium sulfate (98.0%), and all substrate for ester derivatives were purchased from Sigma-Aldrich and used without any further purification. All solvents were obtained from commercial sources and were distilled with appropriate reagents prior to use it. In the present approach, catalyst zinc sulfamate (Zn(SO3NH2)2 was prepared by using stoichiometry (2:1) amount of sulfamic acid (NH3SO3) and zinc oxide (ZnO). The obtained final zinc sulfamate (Zn(SO3NH2)2 powder was directly used as catalyst for the preparation of benzimidazole …show more content…

To this solution, a known amount of catalyst Zn(NH2SO3)2 (10 % mole) was added carefully. The resulting reaction mixture was then heated at 80oC reaction temperature with constant vigorous stirring using magnetic stirrer. The reaction progress was monitored by the thin layer chromatography (TLC). After completion of the reaction indicated by TLC (TLC solvent system; CH2Cl2 and MeOH (90:10)), the reaction mixture was cooled at room temperature and then poured into ice-water. The reaction gave white solid precipitate in the ice-cold water. The precipitated solid was filtered out washed with ice-water three times and further purified by recrystallization with hot ethanol. In addition, purification of product was carried out by passing sample through a short column of silica gel whenever it is necessary. The obtained pure products then examine and confirmed by further characterization using 1H and 13C NMR spectroscopy and elemental analysis. All the melting points of prepared compounds were determined in open capillary tubes and are in corrected. The FT-IR spectra were recorded on a Perkin-Elmer spectrophotometer using KBr pellets. 1HMR spectra were recorded on Varian Gemini (200 MHz) spectrometer using DMSO-d6 as solvent and TMS as internal standard.13C-NMR spectra were recorded on 50 MHz in DMSO-d6 solvent, in δ ppm. All chemical shifts values

Get Access