Aim and Objective:
Nowadays, the design, synthesis and application of magnetically nanocomposite
systems have attracted the attention of numerous scientists. The huge surface area and magnetic characteristic
of nanoparticles as well as the inherent potentiality of the used metal species, makes them susceptible to have
different reactivity in chemical reactions. In this context, we therefore encouraged to prepare a new design of
magnetic nanocatalysts as CuFe2O4@SiO2@AAPTMS@Ni(II) and CuFe2O4@SiO2@AAPTMS@Cu(II)
followed by monitoring of their catalytic activities towards reduction of nitroarenes with NaBH4.
Materials and Methods:
Magnetically nanoparticles of CuFe2
O4@SiO2@AAPTMS@Ni(II) and
CuFe2O4@SiO2@AAPTMS@Cu(II) were prepared through a four-step procedure: i) preparation of CuFe2O4
MNPs, ii) coating of CuFe2O4 nucleus by silica-layer using tetraethyl orthosilicate (TEOS), iii) layering of
CuFe2O4@SiO2 MNPs with [3-(2-aminoethylamino)propyl] trimethoxysilane (AAPTMS), and iv) the
complexation of CuFe2O4@SiO2@AAPTMS MNPs with an aqueous solution of Ni(OAc)2·4H2O or
Cu(OAc)2·H2O.
Results:
The catalytic activity of CuFe2O4@SiO2@AAPTMS@Ni(II) and the Cu(II)-analogue towards
reduction of nitroarenes with NaBH4 was studied. The examinations resulted that using a molar ratio of 1:2 for
ArNO2 and NaBH4 in the presence of 20 mg of nanocomposites in H2O under reflux conditions reduces various
aromatic nitro compounds to arylamines in high yields.
Conclusion:
The immobilization of Ni(II) and Cu(II) species on silica-layered CuFe2O4 was investigated.
Magnetically nanoparticles of CuFe2O4@SiO2@AAPTMS@Ni(II) and the Cu(II)-analogue showed the perfect
catalytic activity towards reduction of nitroarenes with NaBH4 in H2O. All reactions were carried out within 2–
15 min to afford aniline products in high yields.
In this work, a series of new dioximes (DASOX) 2(a-c) and diamines 3(a-c) derivatives were successfully synthesized. The bisaldehydes 1a was first prepared by reaction of 5-bromo-2-hydroxy benzaldehyde with 2,3-dibromo propanol in the presence of sodium hydroxide in reflux conditions. The reaction of various bisaldehydes 1(a-c) with hydroxylamine hydrochloride in an alcoholic solution in the presence of sodium hydroxide results dioximes 2(a-c) in higher yields. Finally, diamines 3(a-c) was generated by the reduction of dioximes 2(a-c) with LiAlH4 in dry THF. All the newly synthesized compounds characterized by melting point, TLC, elemental analysis, FT-IR, 1 H NMR, 13 C NMR and Mass spectroscopy.
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