10.1002/asia.201900878
Chemistry - An Asian Journal
FULL PAPER
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Experimental Section
Generalized synthesis of N-TiO2 hollow spheres. In a typical synthetic
procedure, to a 30 ml TPCC solution
[18]
(obtained from 0.01 mole, 3ml,
titanium isopropoxide), 0-50 ml of 30% NH4OH solution was added under
constant stirring and final volume of the solution was made up to 90 ml by
adding deionized water. Then, 33 ml of this clear solution mixture was
transferred to a 50 ml Teflon lined stainless steel autoclave, sealed
properly and transferred to a pre-heated electric oven at 120 oC for 18 h.
The resultant precipitate was filtered, washed with de-ionized water
followed by ethanol and dried in ambient conditions overnight. Finally the
dried materials were calcined at 400°C for 2 h.
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Characterizations. Powder X-ray diffraction patterns were recorded using
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Miniflex-II (FD 41521) powder diffractometer (Rigaku, Japan).
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Morphological determines were performed using JEOL JSM 7100F
scanning electron microscope (SEM) and a JEOL JEM 2100 transmission
electron microscope (TEM). UV-Vis diffuse reflectance spectra (DRS)
were collected on a Shimadzu UV-2550 spectrophotometer. Raman
spectra were recorded using a Raman spectrometer (NICOLET ALMECA
XR) with a 532 nm laser beam. ESCALAB 250 XPS System with a
monochromatic Al Kα (150 W) source was used to record the X-ray
.
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photoelectron spectra (XPS). PL recorded on
a Horiba Jobin
spectrophotometer. For sectioning the hollow sphere through microtomy
on LEICA EM UC6, the synthesized hollow spheres were embedded in
spurr resin and polymerized by heating at 80 °C for 12 h in air oven.
General synthetic procedure for the synthesis of N-hydroxyimide
esters from N-hydroxyimide (NHI) and alcohol under visible light. In
a typical procedure, 0.2 mmol NHI, 0.4 mmol alcohol, 2 mL acetonitrile
(solvent) and 0.8 mmol TBHP were taken in a 15 mL reaction tube. The
reaction tube was sealed by a septum and filled with oxygen ballon and
then, transferred to a photocatalytic reaction chamber. The reaction
mixture was irradiated by 40W CFL lamp under constant stirring from 18-
24h. After completion of the reaction, the catalyst was separated by
filtration, and the organic layer was diluted with ethyl acetate and washed
with water. The organic part was dried over Na2SO4 and evaporated under
reduced pressure. The crude product was purified by column
chromatography by using an eluent mixture of EtOAC: Hexane.
General procedure for one pot the synthesis of amide and ester:
After 18h reaction of NHI and alcohol under visible light, the light was
switch-off, 3.0 equivalent amine or alcohol was added in the reaction
mixture and stirring was continued for another 2h. After completion of the
reaction, the reaction mixture was poured into H2O (20 ml) and extracted
with ethyl acetate (3×20 ml). The combined organic layer was washed
with brine (30 ml) and dried over Na2SO4. The solvent was removed
under reduced pressure, and the crude reaction mixture was purified by
flash column chromatography using hexane /ethyl acetate as an eluent
to isolate the desired product. The NHI was also recovered for re-use.
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CSIR-CSMCRI Communication No. 035/2019. The authors
acknowledge SERB, India (EMR/2014/001219) for financial
support. The authors acknowledge Dr. Biswajit Ganguly of
CSMCRI for his help and suggestions. The authors also
acknowledge ADCIF of CSIR-CSMCRI for providing instrumental
facilities.
Keywords: Nitrogen-doped TiO2 • hollow spheres • active ester
• N-hydroxyimide • photocatalysis
14 C. Gao, Y.-Q. Peng, L.-H. Hu, L.-E Mo, X.-X. Zhang, T. Hayat, A.
Alsaedi and S.-Y. Dai, Inorg. Chem. Front., 2018, 5, 2284-2290.
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