R. Zhiani et al.
was then dispersed in 15 mL of THF. After magnetically
stirring them at room temperature for 2 h, 6 mmol of cya-
nuric chloride (1.1 g) was added to the solution and the
mixture was stirred again at room temperature for a fur-
3 Results and Discussion
FeNi /KCC-1/APTPOSS/TCT/PVA/Cu(II) MNPs were
3
synthesized through a multistep procedure as illustrated in
ther 16-h period. Ultimately, the synthesized NPs (FeNi /
Scheme 2. FeNi /KCC-1/APTPOSS MNPs were treated
3
3
KCC-1/APTPOSS/TCT) were separated from the reaction
mixture by applying an external magnetic field, washed
several times with water and ethanol, and dried at 70 °C
for 4 h.
with (3-chloropropyl) trimethoxysilane to produce FeNi /
3
KCC-1/APTPOSS-Cl MNPs, which were then allowed to
react with 3-(3-hydroxy-propylamino)-propan-1-ol. The
TCT reaction with FeNi /KCC-1/APTPOSS-N(OH) MNPs
3
2
in the intermediate resulted in their reactions with PVA and
2
.10 General Procedure for the Preparation
then with Cu (OAc) in THF, which consequently yielded
2
of FeNi /KCC‑1/APTPOSS/TCT/PVA MNPs
FeNi /KCC-1/APTPOSS/TCT/PVA/Cu(II) MNPs.
3
3
The morphologies and structures of the FeNi /KCC-1,
3
1
g of FeNi /KCC-1/APTPOSS/TCT NPs was dispersed in
FeNi /KCC-1/TCT/PVA/Cu(II), and FeNi /KCC-1/APT-
3
3
3
2
0 mL of DMF and then, 0.75 g of PVA was completely
POSS/TCT/PVA/Cu(II) MNPs were further characterized
by transmission electron microscopy (TEM) and field emis-
sion-scanning electron microscopy (FE-SEM). As shown in
Fig. 1a, FeNi /KCC-1 possesses a core of FeNi particles,
dissolved in the solution at 80 °C. FeNi /KCC-1/APTPOSS/
3
TCT/PVA composite was obtained after 6 h of stirring at this
temperature. At the end, the NPs were detached from the
mixture and washed with hot ethanol in a Soxhlet apparatus
for 6 h so as to remove the unreacted starting materials.
Finally, they were dried at 60 °C for 5 h.
3
3
a nonporous silica layer, and silica fibers. The as-prepared
magnetic core–shell silica material of FeNi /KCC-1 with a
3
fibrous structure was uniform and mono-dispersed. Also,
the TEM and FE-SEM images of the highly textured FeNi /
3
2
.11 General Procedure for the Preparation
KCC-1 samples revealed that the samples had spheres of
uniform sizes with wrinkled radial structures and diam-
eters of ~300 nm (Fig. 1a, d). After closely assessing the
images, the wrinkled fibers with a thickness of ~9.0 nm
were found to have grown out of the centers of the spheres,
which were radially arranged in three dimensions. In addi-
tion, open cone-shaped pores were observed to be formed
by the overlapping of the wrinkled radial structures. The
TEM and FE-SEM images further revealed the solid states
of the entire sphere being composed of fibers. Hence, the
mass transfer of the reactants could be facilitated by the hier-
archical open-channel structures, through which the fibers
could gain easier access to the active sites. The FE-SEM and
TEM images of FeNi /KCC-1/TCT/PVA/Cu(II) and FeNi /
of FeNi /KCC‑1/APTPOSS/TCT/PVA/Cu(II) MNPs
3
1
g of FeNi /KCC-1/APTPOSS/TCT/PVA and 0.18 g of Cu
3
(
OAc) (1.0 mmol) were added to 20 mL of THF and the
2
mixture was stirred under reflux conditions. After 4 h, the
formed brown precipitate was separated by using an exter-
nal magnetic field and washed several times with water and
ethanol. Ultimately, the filtered precipitate was dried at
6
0 °C for 3 h.
2
.12 General Procedure for the Catalytic
N‑Formylation of Amines
3
3
First, 50 mL of a glass reactor liner was charged with
KCC-1/APTPOSS/TCT/PVA/Cu(II) MNPs displayed no
1
0 mmol of the amines and 5 mL of 1,4-dioxane inside a
changes to FeNi /KCC-1 morphologies after their modifi-
3
glove box. After adding 18 mg of FeNi /KCC-1/APTPOSS/
cations and they were thus alike (Fig. 1b, c, e, f).
3
TCT/PVA/Cu(II) to the mixture, the Parr reactor was sealed
and removed from the glove box. The reactor was then pres-
surized with CO (1.5 MPa) followed by H (2 MPa) and
It was very important to us that the catalyst be stable. The
mechanical stability of FeNi /KCC-1/APTPOSS/TCT/PVA/
3
2
2
Cu(II) MNPs was examined using FE-SEM. The morphol-
the temperature was enhanced to reflux. After 80 min, the
reactor was cooled by submersion in an ice bath and the
remaining gas was slowly vented. Upon completion of the
reaction, the catalyst was separated by using a magnet to be
further utilized for later recycling experiments. After drying
the resultant crude product over anhydrous sodium sulphate,
the mixture was subjected to Column Chromatography (CC)
through a system of petroleum ether/EtOAc as an eluent
ogy of FeNi /KCC-1/APTPOSS/TCT/PVA/Cu(II) MNPs
3
remained unaffected even after applying the mechanical
compression up to 250 MPa pressure (Fig. 2a). Also, we
conducted a series of experiments to study the effects of
microwave irradiation stability on the morphology of FeNi /
3
KCC-1/APTPOSS/TCT/PVA/Cu(II) MNPs with varied
ratios and no impacts were observed at the power of 700 W
(Fig. 2b). FeNi /KCC-1/APTPOSS/TCT/PVA/Cu(II) MNPs
3
(
6:1) on silica gel.
were found to possess high solvothermal stability as their
structures remained unchanged even after heating them in
1
3