5.0 Materials and Methodologies
5.1 Research Methodologies and Framework
The main research will be carried out in Inorganic Research Laboratory at Universiti Malaysia Sarawak (UNIMAS). All chemical will be purchased from Fluka, Aldrich, or J.T. Baker. All of solvent are purified and dried using standard method. Hydrazone/Carbohydrazone ligand and its transition metal complex will be synthesized and characterized by CHN analyses, UV-Visible, FTIR, and 1H NMR spectral studies. All 1H NMR spectra will be analyzed using Jeol 500 MHz spectrophotometer in CDCL3/DMSO-d6 at Universiti Malaysia Sarawak (UNIMAS). All spectroscopic data, molar conductance, and elemental analysis can be used to determine the molecular structure of transition metal complexes
5.2 Laboratory Work
5.2.1 Synthesis of Hydrazone Ligand
The hydrazone ligand that will be synthesized is acetylpyridinebenzyhydrazone ligand. This ligand will be synthesized by condensation reaction acetylpyridine with benzyhydrazide in ethanol solution and 1:1 mole ratio with removal or water molecule (Azaz et al., 2007).
Scheme 220.127.116.11: Synthesis of acetylpyridinebenzyhydrazone ligand
5.2.2 Synthesis of Transition Metal Complexes with acetylpyridinebenzyhydrazone ligand
Metal complexes with acetylpyridinebenzyhydrazone ligand can be synthesized by direct reaction of ligand with the metal chlorides in the presence of base. The proposed structure of metal complexes with acetylpyridinebenzyhydrazone is shown in Figure 18.104.22.168 below.
Figure 22.214.171.124: Metal complexes of acetylpyridinebenzyhydrazone ligand
5.2.3 Synthesis of Carbohydrazone Ligand
The carbohydrazone ligand that will be synthesized is thiocarbohydrazone bis-(benzaldehyde). This ligand will be synthesized by refluxing the bezaldehyde and thiocarbohydrazide in absolute ethanol (Dragancea et al., 2010).
Scheme 126.96.36.199: Synthesis of thiocarbohydrazone bis-(benzaldehyde) ligand
5.2.4 Synthesis of Transition Metal Complexes with...
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