Schiff's Base Lab Report

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SYNTHESIS, CHARACTERIZATION OF SOME SCHIFF’S BASES DERIVED FROM PHENYLHYDRAZINE. NASIRA NIYAZ SURVE*, RASHMI SHANKAR, KABITA SAUD, RAHUL GUPTA, SHANKERDUTT PANDEY,SATU T CHAVHAN, R P CHAVAN.

Department Of Chemistry, Dnyanasadhana College, Thane.

ABSTRACT: A Schiff's Base is a neutral molecule with an electro pair and contains a carbon-nitrogen double bond. This class of compounds was discovered in 1864 by Hugo Schiff. The condensation reactions of an aromatic aldehyde and aromatic amines carried out efficiently in a solvent medium.The formation of Imines or Azomethine are carried out without catalyst using ethanol as solvent. In this method, yields are high, reactions are fast and products are isolated easily
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Metal complex Schiff's bases have also been used in oxidation reaction. The great deal of work has been reported on the complexation of metal ions with Schiff's bases for the study of structure and stability of the complexes. The catalytic effect of hydrogen, hydroxyl and metal ions on the formation and hydrolysis of imines have been studied, In the present work we reported here kinetic study and formation of Schiff's bases using Phenylhydrazine and p-nitroaniline in ethanol medium.
EXPERIMENTAL
Synthesis of Schiff's Base Ligand:

Step-I: Preparation of Schiff's base: Take Salicaldehyde (0.9mmol) with Phenylhydrazine (1.5mmol) in ethanol reflux the reaction mixture for one and an hours and in between take TLC, for the progress of the reaction. After completion of the reaction the hot solution was poured into ice-cold water. Then, the product was filtered under suction and washed with distilled water. The product obtained was yellow coloured solid, were dried at ambient temperature and recrystallised with ethanol.
Yield range 70-75%, Melting
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This reaction is refluxed in a waterbath for two hours and their volume were reduced to 70% of it’s original volume and residue was obtained. The coloured product obtained was filtered under suction, washed with ethanol. The product were recrystallized from ethanol. Their yields ranges from 50-55%, the product obtained were pinkish colour and melting point was 2020C. Step-III: Synthesis of Cr(II) Complexes: The Schiff's base complexes were synthesized by mixing the Schiff's base (1.5 g) in ethanolic solution of Chromium chloride [CrCl2]. This reaction is refluxed in a waterbath for two hours and their volume were reduced to 70% of it’s original volume and residue was obtained. The coloured product obtained was filtered under suction, washed with ethanol. The product were recrystallized from ethanol. Their yields ranges from 50-55%, the product obtained were light green colour and melting point was 2100C.

Step IV: Synthesis of Pb(II) Complexes: The Schiff's base complexes were synthesized by mixing the Schiff's base (1.5 g) in ethanolic solution of Lead nitrate[Pb(NO3)2]. This reaction is refluxed in a waterbath for two hours

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