ChemCatChem
10.1002/cctc.202001041
FULL PAPER
added with an energy-dispersive X-ray spectrometer (EDAX, r-
completion, the reaction mixture was allowed to cool to room
temperature, and the catalyst was separated by magnet. Then
the reaction mixture was extracted with ethyl acetate and
washed with a saturated solution of potassium carbonate. The
organic layer was dried over anhydrous sodium sulfate and
concentrated under vacuum. The crude product was purified
with silica gel column chromatography using hexane and ethyl
acetate to get the corresponding amide.
TEM SUTW). The surface area was measured on
a
Quantachrome Autosorb-1 apparatus. The elemental analyses
were carried out on a Flash EA 112 Thermo Finnigan elemental
analyzer. ICP-AES was measured on a Thermo Jarrell Ash
Trace Scan analyzer. H and 13C NMR spectra were recorded on
1
AVH
D 500 Advance III HD 500 MHz, One Bay NMR
Spectrometer of Bruker Bio Spin International.
Synthesis of Ni-Ni PBA.[32] Ni(OAc)
.4H O (1 mmol) and tri-
2 2
sodium citrate (0.38 mmol) was dissolved in 20 mL of distilled
water and stirred for 10 minutes to form the solution A.
Acknowledgements
2 4
K [Ni(CN) ] (1 mmol) was dissolved in 20 mL distilled water and
This work is financially supported by CSIR (grant no.
stirred for 10 minutes to form the solution B. The solution B was
added to solution A at a time and stirred for five minutes. Sky
blue precipitate of Ni-Ni PBA started appearing after five minutes.
The solution was aged for 24 h at room temperature (without
stirring). The precipitate was collected by centrifugation (at
0
1(2977)/19/EMR-II), Govt. of India.
Keywords: Metal-organic framework • Mott-Schottky catalyst •
NiO@Ni nanoparticles • heterogeneous catalysis • amidation
reaction •
12000 rpm for 10 minutes) and washed five times with water and
finally with acetone. The obtained precipitate was dried at 60 °C
in a hot air oven overnight.
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was ground in a mortar pestle to get a fine powder. The powder
was placed in a crucible boat and heated at 350 °C in the air for
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h (in a tubular furnace with heating rate: 3 °C/min from 35 °C).
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Synthesis of NiO-Ni from Ni(OAc)
powder was taken in crucible boat and annealed in air at 350 °C
heating rate 3 °C/min) for 1 h. The furnace was allowed to cool
down to room temperature. As obtained, the black color powder
was denoted as NiO-Ni.
2 2 2 2
.4H O. Ni(OAc) .4H O
(
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Synthesis of Ni@C from Ni-Ni PBA.[34] The fine powder of Ni-
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Ni PBA (100 mg) was placed in a crucible boat then subjected to
pyrolysis at 700 °C in the nitrogen atmosphere for 30 min (in a
tubular furnace with heating rate: 3 °C/min). The furnace was
allowed to cool down to room temperature. The black powder
was collected and denoted as Ni@C.
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Sample preparation for the characterization of the catalysts.
TEM: ~2 mg catalyst was dispersed in 1 mL of ethanol and
sonicated for 5 min. The suspension was drop casted on a TEM
grid and dried under the IR lamp for 10 min.
SEM: The catalyst powder was deposited on a glass surface
and gold-coated before recording SEM.
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[
7]
PXRD: Powder was taken on a circular Si-plate and a glass
piece was used to press it, resulting in a homogeneous
distribution. The sample on Si-plate was mounted on
diffractometer.
IR: A small amount of powder sample was sprinkled on the
a
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General procedure of amide synthesis.
equiv.), amine (1 mmol, 1 equiv.), TBHP (4 mmol), and
NiO@Ni (5 mg) were added to a round bottom flask containing
,4-dioxane (1 ml). The reaction was refluxed at 60 ⁰C for 8
Aldehyde (1 mmol,
1
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1
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hours with stirring under nitrogen atmosphere. The reaction was
monitored for completion by thin-layer chromatography. After
2
6
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