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4.2 | General Procedure for the synthesis
of MCM‐41 modified by 2‐Methoxy‐1‐
phenylethanone (2‐MPE@MCM‐41)
MCM‐41 was prepared according to the process as
described in a literature.[55] Initially, MCM‐41 (2 g)
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was
added
into
a
suspension
of
3‐
Aminopropyltrimethoxysilane (0.9 ml, 5 mmol) in dry
toluene, and the reaction mixture was stirred at reflux
for 48 h under N2 gas. After cooling, solid was isolated
from the solvent by filtration and washed with toluene
and CH2CL2 (4 × 15 ml) and dried in vacuum at 140 °C
for 5 h. The dried white solid was suspended in a solution
of 2‐Methoxy‐1‐phenylethanone (1.35 ml, 10 mmol) in
ethanol (20 ml). The mixture was refluxed for 24 h under
N2 gas. After cooling, the reaction mixture was filtered
and washed several times with ethanol and dichlorometh-
ane and dried in vacuum to afford 2‐MPE@SiO2.
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4.3 | General procedure for synthesis of
Cu(II)‐2‐MPE@MCM‐41
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The obtained 2‐MPE@MCM‐41 was dispersed in 15 ml
ethanol and a solution of Cu(OAC)2.H2O (2 mmol)
was added dropwise into this mixture under stirring and
was refluxed for about 15 h. Next, the solid product was
separated by filtration and washed with ethanol and
acetone and dried in room temprature.
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4.4 | General procedure for C−S coupling
reaction by Cu(II)‐2‐MPE@MCM‐41
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[16] A. Sujatha, A. M. Thomas, A. P. Thankachan, G. Anilkumar,
A mixture of aryl halide (2.0 mmol), thiourea (1.0 mmol),
KOH (3.0 mmol), Cu(II)‐2‐MPE@MCM‐41 (0.10 mmol Cu)
and 4 ml of DMF:H2O in a round bottom flask equipped
with a condenser was stirred at 130 °C under air for
12 h (for aryl iodide). The reaction progress was con-
trolled by the TLC. After completion of the reaction, cata-
lyst was removed by filtration. Then, separated
nanocatalyst washed by ethyl acetate and water, dried
under vacuum at 60 °C and reused for next runs. Then
the filtrate was extracted with ethyl acetate and the
organic layer was dried over CaCl2. The solvent
was removed under vacuum, and the purified product
was separated by silica gel column chromatography
(n‐hexane:EtOAc, 9:1).
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ACKNOWLEDGEMENTS
We would like to thank the Isfahan University of
Technology (IUT), Islamic Republic of Iran.
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2010, 352, 119.