Synthesis of cobalt (II) complex with new ligand di (furanyle methylene hydrazono) 1.2- di acetyle hydrazine
Study of the synthesis of complexes of diacetylhydrazine with hydrazine hydrate. Carrying out the reaction of the ligand with cobalt in the presence of salts of metal chloride and furfural. Condensation of diacetylhydrazine with hydrazine monohydrate.
| Рубрика | Химия |
| Вид | статья |
| Язык | английский |
| Дата добавления | 15.01.2021 |
| Размер файла | 838,5 K |
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University of Al-Bass
Department of "Inorganic Chemistry"
Faculty of "Natural Sciences"
Synthesis of cobalt (II) complex with new ligand di (furanyle methylene hydrazono) 1.2- di acetyle hydrazine
Hanan Al-Umar, Postgraduate student 3 years,
Al-Khadr Mohamed Mudar,
Candidate of Chemical Sciences, Professor
Syria, Homs
Annotation
A new ligand (L) = [(di Furanyle Methylene hydrazono) 1,2- diacetylehydrazine was synthesized by condensation of 1,2- di acetylehydrazine with hydrazine hydrate then, add the Furfural.
Then the reaction of this ligand with Cobalt (II) ion werecarried out using metal Chloride salt by the (1:2) molar ration respectively conduced[Co2LCl4].the ligand and complexes wereand studied on the basis of (FT-IR) and (1H-NMR,13C-NMR) .the results were comparative with the proposed structures.
Key words: 1,2-di acetyle hydrazine -Furfural - Hydrazine Hydrate .
Аннотация
Синтез комплекса кобальта (II) с новым лигандом ди (фуранил метилен гидразоно) 1,2- иацетилгидразина
Ханан Ал-Умар, Студент аспирантской подготовки 3- года, факультет «естественных наук» Кафедра «по неорганическая химия» Университет Аль-Басс Сирия, г. Хомс
Аль-Хадр Мохамед Мудар, кандидат химических наук, профессор кафедры «по неорганическая химия» Университет Аль-Басс Сирия, г. Хомс
Новый лиганд (L) = [(дифуранилметилгидразоно) 1,2- диацетилгидр- азин] синтезировали путем конденсации 1,2 -ди ацетилгидразина с гидразингидратом, затем добавляли фурфурол. Затем реакция этого лиганда с кобальтом (II) иона проводили с использованием соли хлорида металла с помощью (1: 2) молярного соотношения соответственно проведенного [Co2LCl4]. Лиганд и комплексы исследовали на основе (FT-1R) и (1Н-ЯМР, 13С-ЯМР). результаты были сопоставимы с предлагаемыми структурами.
Ключевые слова: 1,2-ди ацетил гидразин - фурфурол - гидразин гидрат.
Introduction
Schiff bases have been subject of interest as a resutt of their synthetic accessibility and rich coordination chemistry [1,c.617], These compounds [2,c.2048] and their metal complexes have been reported to exhibit a wide spectrum of biological properties [3,c.4368].During the past two decades, considerable attention has been paid to the chemistry of metal complexes of Schiff bases containing nitrogen and other donor atoms [4,c.2175/5,c.207].
Experimental
Apparatus and chemicals. All the chemicals used were purchased from both Merch and Sigma Aldrich companies and used without further purification. FT-IR spectra was recorded using Jasco Japanese taype (A) Infrared Spectrophotometer Fourier Transform FT-IR- 4100(KBr). spectrum NMR proton and carbon device 400 MHzmodel Bruker by Switzerland company.
Eperimental procedure
Synthesis of the ligand (L): The Schiff base, (L) was prepared by condensation of 1,2-di acetyle hydrazine (1.18gr,10mmol) with hydrazine hydrate (2.5ml) in ethanol 95% (50ml), then adding the furfural (2.5ml).
The mixture was refluxed with stirring for 16h.The precipitated [(di Furanyle Methylene hydrazono)1,2-di acetyle hydrazine] were filtered and recrystallized from ethanol. Ligand as yellow crystals was obtaind with a yield of (53%) and m.p=n0-115°C. synthesis diacetylhydrazine furfural ligand
Synthesis of metal complexes: A solution of ligand (L) (0.15gr, 0.5mmol) in methanol (15ml) was added to a solution of metal cobalt chloride hydrous (0.5*2 mmol) in methanol (10ml), and refluxed for 17h by using a water bath. By cooling the contents, the colored complex separated out in each case. The same was filtered, then washed with ethanol and washed several times with diethyl ether.
Results and Discussion
(13C and1HNMR) spectroscopic measurements: The (13C and 1H-NMR) spectroscopic measurement of (L) Schiff base are given in table 1.
Table1. Explanation of (13C and 1H-NMR) ppm of the ligand (L).
|
No |
13C-NMR(8 ppm ) |
No |
1H-NMR(8 ppm) |
|
|
C1 |
150.89 |
1 |
4.48) 1H,s ( |
|
|
C2 |
21.22 |
2 |
2) 3H,s( |
|
|
C3 |
149.40 |
3 |
(8.19) 1H,s |
|
|
C4 |
145.77 |
4 |
6.55-6.56) 1H,d( |
|
|
C5,6 |
112.27 |
5 |
(6.18-6.19) 1H,dd |
|
|
C7 |
116.68 |
6 |
7.25-7.26) 1H,d( |
Figure l. 1H-NMR spectrum of the ligand (L) [(di Furanyle Methylene hydrazono)1,2-di acetyle hydrazine] in Cloroform.
Figure2. 13C-NMR spectrum of the ligand (L) [(di Furanyle Methylene hydrazono)1,2-di acetyle hydrazine] in Cloroform.
Infrared Spectra: The infrared spectra for the present compounds taken in the range 400-4000 cm-1 help to indicate regions of absorption vibrations. The main stretching modes are for v(C=N)i, v(C=N)2 and v(C-O-C).
Figure 3. IR absorption spectra of ligand (L
Figure 4. IR absorption spectra of [Co2LCE].
Table 2.
Conductivity and melting point of the ligand and complex.
|
compounds |
M.P(°C) |
color |
Yield |
conductivity Ps |
v(C=N)1 cm-1 |
v(C=N)2 cm-1 |
v(C-O-C) cm-1 |
Geometry |
|
|
L |
110-115 |
Yellow |
53% |
0 |
1641 |
1575 |
949 |
||
|
[Co2LCl4] |
>250 |
Dark red |
90% |
70 |
1638 |
1543 |
927 |
Tetrahedral |
Conclusion
The synthesise of a new ligand (L) di(furanyle Methylene Hydrazono)1,2-di acetyle hydrazine was carried by condensation of 1,2-di acetyle hydrazine with hydrazine mono hydrate ,Then add furfural to getting ligand (L).Then the reaction of this ligand with Cobalt(II) ion were carried out using metal Chloride salt by the (1:2) molar ration respectively conduced. [Co2LCl4]
References
1. Aslantas. M, Kendi. E, Demir. N, A.E. Sabik. A.E, Tumer. M and Kertmen. M.Synthesis, spectroscopic, structural characterization, electrochemical and antimicrobial activity studies of the Schiff base ligand and its transition metal complexes // Journal of Spectrochimica Acta Part A.-2009.- № (74).-C.617-624.
2. Xu. S.P, Shi.L, Lv. P.C, Fang. R.Q. and Zhu. H.L. Synthesis and anti bacterial activities of metal(II) complexes with Schiff bases drived from 3.5- diiodosalicylaldehyde // Journal of Coordination Chemistry.-2009.- № (62).-C.2048.
3. Nejo. A.A, Kolawole. G.A, Dumbele. M.C. and Opoku. A.R. spectral, magnetic, biological, and thermal studies of metal(II) complexes of some unsymmetrical Schiff base // Journal of Coodination Chemistry.-2010.- № (63).-C.4367-4379.
4. Djebbar. S.S, Benali. B.O. and Deloume. J.P. Synthesis, characterization and electrochemical behavior of copper(II) complexes with linear and tripodal tetradentate ligand derived from Schiff base // Journal of Polyhedron.-1997.- № (16).-C.2175-2182.
5. He. L, Gou. S. H. and Shi. Q. F. The formation of a Schiff base intermediate a nickel(II) complexes of an asymmetric tripodal ligand //Journal of J.Chem Chystallogr.-1999.- № (29).-C.207-210.
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