ISSN 10703284, Russian Journal of Coordination Chemistry, 2015, Vol. 41, No. 7, pp. 451–455. © Pleiades Publishing, Ltd., 2015.
The development of processes for oxidation of ole
fins is a goal that has long been pursued. Highvalent
molybdenum complexes have attracted continuing
attention due to their important practical applications
as catalysts in the ammoxidation of propene, the sul
foxidation and epoxidation of olefins, etc. [1–7]. The
ability of molybdenum to form stable complexes with
oxygen and nitrogencontaining ligands led to the
development of molybdenum Schiff base complexes
which are efficient catalysts both in homogeneous and
heterogeneous reactions [8–13]. Recently, we have
reported some metal complexes with Schiff bases, and
their biological aplications [14–16]. As a continuation
of the work on the exploration of new catalytic materials
based on Schiff base complexes, in this paper, a new
where L =
zylidene)4hydroxybenzohydrazide), is described.
Materials and instrumentations.
obtained by published method . The remaining
reagents were supplied by Merck and Fluka, and were
employed without further purification. IR spectra
were recorded on a Shimadzu Varian 4300 spectro
H NMR spectrum of the complex was
recorded on a Bruker FTNMR 300 MHz spectrome
as solvent. The electronic spec
The article is published in the original.
trum was recorded on a Shimadzu UV
spectrophotometer (Model 2101 PC). Elemental
analyses (C, H and N) were performed using a Carlo
Erba Model EA 1108 analyzer. GC analyses were per
formed on a Shimadzu GC2010 gas chromatograph.
Syntheses of I.
To a solution of 4diethylaminosal
icyldehyde (1 mmol) in 25 mL methanol was added a
solution of 4hydroxybenzohydrazide (1 mmol) in
15 mL methanol, and the reaction mixture was heated
at reflux for 1 h. Then a solution of
(1 mmol) in 15 mL methanol was added dropwise
under stirring. The solution color changed immedi
ately to yellow. After the reflux was continued for
30 min, three quarter of the solvent was evaporated.
The solid product was filtered and washed with meth
anol (67% yield). Single crystals, suitable for Xray
diffraction, were obtained by slow evaporation of the
methanolic solution of the product.
, 2971, 2923,
2857, 1612, 1579, 1507, 1402, 1350, 1245, 1136, 1016,
935, 887, 835, 787, 711, 650. Electronic absorption
spectrum in acetonitrile (
, nm (
(10232), 346 (13870), 472 (12880).
(300 MHz; DMSO
, ppm): 10.06 (s., 1H), 8.54
(s., 1H), 7.78 (d., 2H), 7.40 (d., 1H), 6.83 (d., 2H),
anal. calcd., %: C, 47.02; H, 4.78; N, 8.66.
Found, %: C, 46.86; H, 4.89; N, 8.82.
Synthesis, Structure, and Catalytic Oxidation
of a Molybdenum(VI) Complex [MoO
H. Y. Liu
*, L. Q. Zang
, and J. L. Lv
School of Chemistry and Chemical Engineering, Guangdong Pharmaceutical University, Zhongshan, 528453 P.R. China
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, 510006 P.R. China
Received December 9, 2014
—A new molybdenum(VI) complex, [MoO
OH)(L)] (L =
benzylidene)4hydroxybenzohydrazide), was prepared and characterized by spectroscopy methods and sin
gle crystal Xray diffraction (CIF file CCDC no. 1038153). The crystal of the complex, C
crystallizes in the triclinic space group with unit cell dimensions
= 1025.9(2) Å
= 1.060. The Mo atom in the complex is in an octahedral coordination with phenolate O, imino N,
enolate O atoms of the ligand L, and one oxo O in the equatorial plane, and with one methanol O and the
other oxo O in the axial sites. Crystals of the complex are stabilized by hydrogen bonds. The complex was
studied for its catalytic oxidation property on some olefins, with
butyl hydrogen peroxide as oxidant.