Synthesis Of P-Hydrazone And Resacetophenone Report

2.1 Synthesis of p-Toulichydrazone and Resacetophenone Schiff base (RAPPTH): p-Toluic hydrazide (1.5018g) and Resacetophenone (2,4Dihydroxyacetophenone)(1.5215g) were dissolved in methanol and Refluxed in the presence of few drops of acetic acid for 7 hours on water bath with constant stirring. The resultant mixture was transferred in a china dish and allowed to cool naturally. Light brown crystals were obtained. The compound was recrystalized from water. The % of yield was 80% and melting point of the compound was 218-2200C.

Scheme: Synthesis of RAPPTH

2.2 Synthesis of Mn (II), Co (II), Ni (II) and Cu (II) metal complexes of p-Toluic hydrazone and Resacetophenone Schiff base (RAPPTH): The reagent p-Toluic hydrazone and Resacetophenone(2,4dihydroxyacetophenone) Schiff base was dissolved in 40ml of 50% methanol and Mn (II), Co (II), Ni (II) and Cu (II) metal ions dissolved in 20ml of distilled water, this compounds mixture was stirred for 6 hours in the presence of sodium acetate. Thick Green, Brown, Light yellow and Green colour metal complexes were formed respectively with good yield. These products were washed several times with hot water and cold methanol. Metal
RAPPTH-Co (II): H1 NMR: δ2.61 (s,CH3,3H),2.49(s,CH3,3H),6.40- 7.97 (m,pyH,7H ), 9.98(s, OH.IH), 11.29ppm (s, NH, 1H). IR (KBr): 3480(OH, water), 3227(ph O-H), 1585(C=N), 3349(N-H), 1666 (C=O), 554(M-O), 436 cm-1 (M-N).RAPPTH-Cu (II): H1 NMR: δ2.73 (s,CH3 ,3H),2.50 (s,CH3, 3H), 6.42- 7.95(m,pyH,7H), 10.14 (s,OH.IH), 11.30ppm (s,NH,1H). IR (KBr): 3420(OH, water), 3230(ph O-H), 1609(C=N), 3352(N-H), 1662 (C=O), 639(M-O), 492 cm-1 (M-N). RAPPTH-Mn (II): IR (KBr): 3430(OH, water), 3232(ph O-H), 1596(C=N), 3347(N-H), 1671 (C=O), 616(M-O), 425 cm-1 (M-N). RAPPTH-Ni (II): IR (KBr): 3415(OH, water), 3236(ph O-H), 1606(C=N), 3350(N-H), 1658 (C=O), 637(M-O), 450cm-1