6
JAGADALE ET AL.
spectrometer under prescribed operating conditions. Mass
spectra were recorded with a Shimadzu QP2010 GC–MS.
The materials were analysed by SEM using a JEOL model
JSM with 5 and 20 kV accelerating voltages. Melting points
were determined using MEL‐TEMP capillary melting point
apparatus and are uncorrected. 1‐N‐(ferrocenylmethyl)
triazole was synthesized following a literature procedure.[16]
Cellulose (1) and all other chemicals were obtained from
local suppliers and used without further purification. XPS
was conducted with a KRATOS AXIC 165 equipped with
Mg Kα radiation.
with CH2Cl2 (3 × 20 ml) and dried under vacuum for 48 h
to afford complex 6.
FT‐IR (KBr, thin film, ν, cm−1): 3346, 2900, 1623, 1427,
1383, 1372, 1356, 1316, 1280, 1247, 1235, 1203, 1161, 1111,
1056, 1034, 897, 704, 664, 617, 559, 520. Raman (cm−1):
490, 599, 978, 1086, 1318, 1379, 1487, 1592, 1657, 1786,
2803, 2959, 3146, 3197. Elemental analysis observed (%):
C, 26.59; N, 26.38; O, 42.10; Al, 0.49; Si, 0.45; Fe, 0.95;
Ag, 3.04. Loading: 0.28 mmol of Ag per gram of cellulose.
4.5 | General method for synthesis of diaryl ethers
A mixture of phenol (1.2 mmol), aryl halide (1 mmol),
K2CO3 (2 eq.) and complex 6 (50 mg) in toluene (5 ml)
was stirred at 80°C. The progress of the reaction was moni-
tored by TLC. After completion, the reaction mixture was fil-
tered to remove insoluble catalyst. Evaporation of solvent in
vacuo followed by column chromatography over silica gel
using petroleum ether–ethyl acetate afforded pure products.
4.1 | Preparation of Cell–Al2O3 composite (2)
A blend of microcrystalline cellulose 1 (15 g), aluminium
chloride hexahydrate (15 g) in water (200 ml) was stirred
for 12 h. The mixture was subsequently filtered and resultant
solid was exposed to ammonia. Finally, it was washed with
water and dried under vacuum at room temperature to afford
Cell–Al2O3 composite 2. The amount of aluminium was
determined by calcining 0.300 g of 2 to 600°C for 8 h and
the residue weighed as Al2O3, which was found to be
3.27 wt%, corresponding to 0.69 mmol g−1 aluminium.
ACKNOWLEDGMENTS
We gratefully acknowledge the Indian Institute of Sciences
(IISc), Bangalore and Sophisticated Analytical Instrumental
Facility, Indian Institute of Technology, Madras (IITM) for
providing spectral facilities and Shivaji University, Kolhapur
for providing a Golden Jubilee Fellowship.
4.2 | Preparation of chloropropylcellulose (3)
A mixture of 2 (10.0 g) and (3‐chloropropyl)triethoxysilane
(9.6 ml, 40.0 mmol) in 25 ml of toluene was refluxed in an
oil bath. After 24 h, the reaction mixture was cooled, and the
product was filtered and washed with toluene (3 × 5 ml) and
dried under vacuum at room temperature for 8 h to afford 3.
FT‐IR (KBr, thin film, ν, cm−1): 3366, 2898, 1623, 1427,
1335, 1204, 1160, 1109, 1056, 1032, 707, 667. Loading:
0.59 mmol of functional group per gram of cellulose.
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4.3 | Preparation of [CellFemTriaz]Cl (5)
A mixture of 3 (7.0 g) and 1‐N‐ferrocenylmethyl‐1,2,4‐triazole
(4; 3.76 g, 14 mmol) in DMF (25 ml) was heated at 80°C in an
oil bath. After 72 h, the solid was filtered, washed with DMF
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3142, 3176. Elemental analysis observed (%): C, 30.03; N,
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0.15 mmol of functional group per gram of cellulose.
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A mixture of 5 (5.0 g) and Ag2O (1.70 g) in CH2Cl2 (40 ml)
was stirred at room temperature for 48 h in the dark. After-
wards, the mixture was filtered and the residue was washed