Synthesis and characterization of co-doped fly ash catalyst for chalcone synthesis

Article abstract of DOI:10.14233/ajchem.2019.22053

A series of solid base fly ash hybrid materials were synthesized by doping alkali, alkaline earth metals with nitrogen, separately using co-precipitation process, combined with surfactant incorporating method. The catalysts were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and photoluminescence spectroscopy. Results revealed that the co-doped hybrid materials are highly stable with particle size in the range of 40-60 nm. The surface basicity of fly ash was upraised by increased hydroxyl content by doping with alkali, alkaline earth metals with nitrogen. The basicity of hybrid material was measured by liquid phase, solvent free, single step condensation of 4-chlorobenzaldehyde and acetophenone giving higher conversion rate and selectivity of desired product chalcone. This conversion showed that the fly ash based hybrid material has sufficient basic site, responsible for the catalytic activity.

Full text of DOI:10.14233/ajchem.2019.22053

Asian Journal of Chemistry; Vol. 31, No. 10 (2019), 2165-2172
A
SIAN
J
OURNAL OF HEMISTRY
C
https://doi.org/10.14233/ajchem.2019.22053
Synthesis and Characterization of Co-Doped Fly Ash Catalyst for Chalcone Synthesis
1
1
2
3,*
U.G. GHOSHIR , S.R. KANDE , G.G. MULEY and A.B. GAMBHIRE
1Department of Chemistry, New Arts, Commerce and Science College, Ahmednagar-414001, India
2Department of Physics, Sant Gadge Baba Amravati Univeristy, Amravati-444602, India
3Department of Chemistry, Shri Anand College, Pathardi-414102, India
*Corresponding author: Fax: +91 2428 223033; Tel: +91 2428 222736; E-mail: abg_chem@ymail.com
Received: 6 March 2019; Accepted: 15 April 2019; Published online: 30 August 2019;
AJC-19517
A series of solid base fly ash hybrid materials were synthesized by doping alkali, alkaline earth metals with nitrogen, separately using co-
precipitation process, combined with surfactant incorporating method. The catalysts were characterized by X-ray diffraction, scanning
electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and photoluminescence spectroscopy. Results
revealed that the co-doped hybrid materials are highly stable with particle size in the range of 40-60 nm. The surface basicity of fly ash
was upraised by increased hydroxyl content by doping with alkali, alkaline earth metals with nitrogen. The basicity of hybrid material was
measured by liquid phase, solvent free, single step condensation of 4-chlorobenzaldehyde and acetophenone giving higher conversion rate
and selectivity of desired product chalcone. This conversion showed that the fly ash based hybrid material has sufficient basic site,
responsible for the catalytic activity.
Keywords: Chalcone, Co-doped fly ash, Solid base catalyst.
ash is generated during the combustion of coal in coal-fired
power stations, containing a variety of metal oxides in the order
SiO2 > Al2O3 > Fe2O3 > CaO > MgO > K2O > Na2O >TiO2, if
not put to beneficial use, is a recognized environmental pollutant
[27]. Previously, several fly ash based heterogeneous catalysts
such as CaO have been employed as a recyclable solid base
catalyst for the Knoevenagel condensation reaction [28], CaO
catalyst for the transesterification of soybean oil [29], sulfated
zirconia for benzylation [30], cerium triflate for Friedel-Crafts
acylation [27]. However, most of the above reported research
work claims chemical activation of fly ash with acid and base
in solid state.
Recently, it was found that co-doped metal oxides exhibited
high surface basicity and variation in basic sites in the comp-
osite materials depends on nature of dopants [31-33]. Hence,
it may be possible to design synergistically generated solid
base catalyst by chemical activation of fly ash with co-dopant.
In the present work, we find that doping of alkali, alkaline
earth metals with nitrogen, separately on fly ash shows higher
conversion rate and selectivity of desired product chalcone.
INTRODUCTION
Fly ash (FA) has great deal of interest towards their appli-
cations particularly in production of most industrially impor-
tant fine chemicals [1]. Traditionally, the synthesis of chalcones
is carried out via Clasien-Schmidt condensation either in basic
or in acidic medium under homogeneous conditions such as
NaOH [2-11], KOH [12-15], Ba(OH)2 [16-18]. The acid
catalyzed methods include the use of BF3 [19], HCl [20,21],
TiCl4 [22]. Recently, chalcone synthesis has been achieved
employing Suzuki reaction [23], sulfonic acid from bamboo
[24], acidic ionic liquids [25] and graphene acid [26]. Use of
these acid or bases requires an extra step to separate them from
the reaction mixture and their regeneration is also not possible
in normal conditions. The production of undesired polymeric
byproducts lowers the yield of the desired product.
With the increasing public concern over environmental
degradation and future resources, it is of great importance for
chemists to come up with new approaches that are less hazar-
dous to environment and human being. To overcome these
problems one approach is to use fly ash as green medium. Fly
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2166 Ghoshir et al.
Asian J. Chem.
Mg Kα (hν = 1253.6 eV) radiation were used as the excitation
source. Photoluminescence study was carried out using Hitachi
fluorescence spectrophotometer (F-7000).
Catalytic activity: The activity of synthesized fly ash based
hybrid catalyst were evaluated by condensation reaction between
4-chlorobenzaldehyde and acetophenone by conventional and
non conventional method by Claisen-Schmidt condensation
gives a chalcone ((E)-3-(4-chlorophenyl)-1-phenyl-2-propen-
1-one) as shown in Schemes I and II.
EXPERIMENTAL
Fly ash collected from ParliVaijnath, (Maharashtra, India)
Thermal Power Plant was used as a support material for the
preparation of co-doped hybrid heterogeneous catalyst. All
the chemicals viz., aldehydes, ketones, nitrates of alkali, alkaline
earth metals and ammonia were purchased from Sigma-Aldrich.
Catalyst preparation: The solid base fly ash hybrid mate-
rials were prepared by chemical activation of fly ash with alkali
nitrates and alkaline earth metals and nitrogen, separately by
co-precipitation method, combined with surfactant incorp-
orating method. The activated fly ash (900 ºC), alkali nitrates
and alkaline earth metals mixed with ammonia (source of
nitrogen), separately in the ratio of 2:1:1. The cationic surfactant
cetyltrimethylammonium bromide (CTAB) 10 % (20 mL) in
ethanol was dropped into the above solution. The system was
kept under constant stirring for 12 h and aged for another five
days, followed by drying at 110 ºC and calcined at 400 ºC for
2 h under static condition.
Characterization: X-ray powder diffraction (XRD) patterns
were taken at room temperature using a model D8 BrukerAXS
with monochromatic Cu radiation (40 kV and 30 mA). The
particle size of the sample was calculated from the peak of maxi-
mum intensity (2θ = 26.77º). The microscopic nanostructures
were observed by transmission electron microscopy (TEM;
FEI, Tecnai F30, HRTEM, FEG operated at 300 kV. Surface
morphology and elemental analysis of the samples were carried
out using an energy dispersive spectrophotometer (EDS) (Jeol;
JED-2300). FT-IR spectra were recorded on a Shimadzu-8400
spectrometer in the range of 4000-500 cm-1. X-ray photoelectron
spectroscopy (XPS; ESCA-3000,VG Microtech, Uckfield, UK)
was used to study the chemical composition of the samples.
Non-chromatic X-ray beams of Al Kα (hν = 1486.6 eV) and
Synthesis of chalcone
Conventional method: An equimolecular quantities of
4-cholorobenzaldehyde (2 mmol), acetophenone (2 mmol)
dissolved in 15 mL absolute alcohol in a 100 mL round bottom
flask equipped with refluxing condenser placed on a magnetic
stirrer.About 0.75 g of fly ash based hybrid materials was imm-
ersed into the above solution. The reaction mixture was refluxed
at 120 ºC upto the completion of reaction and it was checked
by TLC on silica gel plates. The reaction product was poured
into the ice-cold water resulting in the formation of crystals,
the crystals were filtered and washed with cold water and then
recrystallized in absolute ethanol.
Microwave irradiation method:An appropriate equimolar
quantity of substituted 4-chlorobenzaldehyde (2 mmol), aceto-
phenone (2 mmol) and fly ash based catalyst (0.75 g) have been
taken in borosil tube and tightly capped. The mixture is exposed
to microwave for 2-3 min in a microwave oven and then cooled
at room temperature. The organic layer has been separated
with dichloromethane which on evaporation yielded the solid
product. The solid on recrystallization with benzene-hexane
mixture gives glittering solid. The insoluble catalyst has been
recycled by washing the solid reagent remained on the filter
by ethyl acetate followed by drying in an oven at 100 ºC for 1 h.
H3C
O
O
O
H
Fly ash based
hybrid catalyst
+
Cl
Cl
4-chlorobenzaldehyde
acetophenone
(E)-3-(4-chlorophenyl)-1-phenylprop-2-en-1-one
Scheme-I: Synthesis of (E)-3-(4-chlorophenyl)-1-phenylprop-2-en-1-one using different fly ash based hybrid materials using conventional
and microwave irradiation method
H3C
O
O
O
H
Ba-N /FA
+
Microwave
Cl
Cl
4-chlorobenzaldehyde
acetophenone
(E)-3-(4-chlorophenyl)-1-phenylprop-2-en-1-one
Scheme-II: Synthesis of chalcone ((E)-3-(4-chlorophenyl)-1-phenylprop-2-en-1-one) using Ba-N/FA catalyzed Claisen-Schmidt condensation
between 4-chlorobenzaldehyde and acetophenone in microwave irradiation method

Vol. 31, No. 10 (2019)
Synthesis and Characterization of Co-Doped Fly Ash Catalyst for Chalcone Synthesis 2167
This recycled catalyst has been made reusable for further
reactions.
BaO at 2θ = 51.83º, 29.66º, 57.74º, 39.53º, 45.92º, 31.72º,
35.31º, 39.32º, 45.23º, 55.21º, 60.77º, 33.36º, 36.95º and
50.51º, respectively. The peaks of co-doped fly ash have been
slightly shifted due to solid solution (marked in trace). The
average particle sizes of the samples were calculated using
Debye-Scherrer formula based on the XRD peak broadening
analysis at 110 peak [30]. The particle size calculated from
XRD data is as large as 70-85 nm for nitrogen doped Li2O/FA,
Na2O/FA, MgO/FA, CaO/FA and as small as 40-60 nm for
SrO/FA, BaO/FA, samples. This apparent fall in particle size
(higher specific surface area) will ensure high catalytic perfor-
mance for the nitrogen doped SrO/FA, BaO/FA, when it is used
for organic transformation.
(E)-3-(4-Chlorophenyl)-1-phenyl-2-propen-1-one: Pale
yellow solid,Yield: 74 %. 1H NMR (250 MHz, CDCl3): δ 8.09-
8.02 (m, 2H), 7.78 (d, J = 15.7 Hz, 1H), 7.67-7.46 (m, 6H),
7.46-7.37 (m, 2H). 13C NMR (63 MHz, CDCl3): δ 190.2, 143.3,
138.1, 136.5, 133.4, 133.0, 129.7, 129.3, 128.8, 128.6, 122.5.
Catalyst regeneration: The spent catalyst in synthesis
of chalcone was washed with acetone, dried in an oven at 110
ºC for 12 h, followed by activation at 250 ºC for 2 h and reused
in further reaction. The regeneration study showed that catalyst
is reusable and there is no considerable change in its catalytic
activity upto 4th reaction cycle.
SEM-EDS, TEM and HRTEM analysis: In order to
further confirm the effect of co-dopant on the particle size, the
particle size of pure fly ash and Ba-N/FA sample were observed
using SEM and TEM, respectively. Fig. 2a showed the SEM
image of pure fly ash is irregular in shape and agglomerated
particles. The activated fly ash revealed that the particle sizes
are in the range of 0.5-0.6 mm. Elemental analysis of pure fly
ash is given in Table-1.
Fig. 2b-c shows TEM and HRTEM images of Ba-N/FA
sample and its corresponding Fourier transfer pattern is also
presented in the inset of Fig 2b. It can be seen that particle
size of co-doped fly ash is about 40 nm. The HRTEM image
of co-doped fly ash (Fig. 2c) also represents presence of highly
crystalline nanoparticles with mesopores.
RESULTS AND DISCUSSION
XRD: To understand phase symmetry in the calcined
samples, a systematic X-ray diffraction study was undertaken.
Fig. 1a shows the XRD patterns of pure and N-doped fly ash,
calcined at 400 ºC for 2 h under static condition. All samples
show sharp peaks at 2θ = 20.97º and 26.77º corresponding to
(111) and (021) phase of monoclinic fly ash [ASTM card No.
86-0680]. The peaks were apparently broad, showing that the
small sized nanocrystalline fly ash was obtained. No peaks
corresponding to doped nitrogen is observed in the pattern. In
case of co-doped fly ash by alkali and alkaline earth metals
with nitrogen, separately (Fig.1b). XRD patterns showed some
additional reflections due to Li2O, Na2O, MgO, CaO, SrO and
(a)
Ba
(b)
N-doped fly ash
Sr
Ba-N/FA
Sr-N/FA
Ba
Ba
Sr
Sr
Sr
Sr
Sr
Na
Ca-N/FA
Mg-N/FA
Ca
Ca
Mg
Na-N/FA
Li-N/FA
Pure fly ash
Li
10
20
30
40
50
60
70
10
20
30
40
50
60
70
2
θ
(°)
2θ (°)
Fig. 1(a-b). XRD pattern of (a) Pure fly ash, N-doped FA; (b) Li-N/FA, Na-N/FA, Mg-N/FA, Ca-N/FA, Sr-N/FA and Ba-N/FA

2168 Ghoshir et al.
Asian J. Chem.
Fig. 2(a-c). (a) SEM image of pure fly ash; (b) TEM image of Ba-N/FA; (c) HRTEM image of Ba-N/FA
TABLE-1
ELEMENTAL COMPOSITION OF PURE FLY ASH FROM EDS (%)
Elements
Wt. (%)
At. (%)
C
35.89
45.28
O
50.63
47.96
Mg
0.18
0.11
Al
4.11
2.31
Si
6.73
3.63
K
0.24
0.09
Ca
0.43
0.16
Ti
0.24
0.08
Fe
0.68
0.18
Cu
0.37
0.09
Zn
0.33
0.08
Zr
0.17
0.03
FT-IR analysis: FT-IR spectrum of pure fly ash (Fig. 3a)
showed the characteristic peaks of silica at 1108, 1661, 562
and 3426 cm-1 [34,35]. The intense peak observed at 1108 cm-1
is attributed to the stretching frequency of Si-O-Si bond. The
peak at 562 cm-1 corresponds to Al-N bond. Band at 1661 and
3426 cm-1 representing the bending mode (δ-O-H) of water
molecule and adsorbed water molecules on the surface. Fig.
3b shows same peaks and band, including one additional peak
at 2340 cm-1 due to carbon impurities. The stretching band for
-NH2 groups, which is usually found in the range of 3400 cm-1,
could not be observed in the spectrum because overlapping of
the band with that of -OH vibration groups [28]. Fig.3c shows
FT-IR spectra of nitrogen, alkali and alkaline earth metal co-
doped fly ash, separately. No additional peaks corresponds to
metals is assigned. The remaining peaks and bands are similar
as shown in (Fig. 3a-b), excluding the broadening in the band
at 3400 cm-1 is observed due to doping alkali and alkaline
earth metals which shows higher basicity associated with doped
fly ash.
XPS study: Fig. 4a-b show general XPS survey of (a)
pure fly ash and (b) Ba-N/FA. Pure fly ash and Ba-N/FA shows
presence of oxygen, carbon, silicon, aluminum and magnesium
elements. Some additional elements such as barium and nitrogen
can be seen in the co-doped sample (Ba-N/FA). Fig. 4c-d shows
high resolution XPS spectra of the O1s region taken on the
surface of fly ash and Ba-N/FA. The O1s peak shows broad-
ening and asymmetry towards the higher binding energy side,
these Peaks are resolved into two component with binding
energy value 530.4 and 533.5 eV for the first and second peak,
respectively. The binding energy of first peak is well matched
(b) N-doped FA
(a) Pure FA
(c)
3402
2340
3406
Ba-N/FA
Sr-N/FA
2355
3426
1652
3446
2052
Ca-N/FA
Mg-N/FA
2349
3396
651
Na-N/FA
Li-N/FA
1519
1633
670
671
3215
1122
877
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm–1)
3500 3000 2500 2000 1500 1000 500
Wavenumber (cm–1)
3500 3000 2500 2000 1500 1000 500
Wavenumber (cm–1)
Fig. 3(a-c). FT-IR spectra of (a) pure fly ash; (b) N-doped fly ash; (c) Li-N/FA, Na-N/FA, Mg-N/FA, Ca-N/FA, Sr-N/FA and Ba-N/FA

Vol. 31, No. 10 (2019)
Synthesis and Characterization of Co-Doped Fly Ash Catalyst for Chalcone Synthesis 2169
(a)
FA
O1s
O1s
(c) FA
O1s
O1s(OH)
C1s
Mg
Si2p
Ca2p
Al2p
12001100 1000 900 800 700 600 500 400 300 200 100
Binding energy (eV)
0
(d) Ba-N/FA
O1s
(b)
Ba-N/FA
Ba3d5
O1s
O1s
O1s(OH)
Si2p
C1s
N1s
Al2p
524
526
528
530
532
534
536
538
540
12001100 1000 900 800 700 600 500 400 300 200 100
Binding energy (eV)
0
Binding energy (eV)
Fig. 4. XPS general survey of (a) pure fly ash; (b) Ba-N/FA; and high resolution XPS spectra of O1s region taken on the surface of (c) pure
fly ash, and (d) Ba-N/FA
with the binding energy of metal-oxides in pure fly ash and
Ba-N/FA, while the second peak is either adsorbed oxygen or
hydroxyl species on the surface, respectively. The chemical
state of catalyst surface is key factor that strongly affect the
catalytic performance of catalyst. The quantitative analysis of
the active cations and anions on the surface of catalyst is impor-
tant factor for evaluation of catalytic activity. In this study,
curve-fitting method was used to calculate the atomic % of
elements [36]. The quantitative analysis results are given in
Table-2. From the quantitative analysis it is found that atomic
% of O2− in Ba-N/FA is higher in comparison with pure fly
ash, that might be due to variation in impurity level create
the charging balance that must be satisfied; therefore more
hydroxide ions are adsorbed on the surface.
Photoluminescence analysis: Photoluminescence spectra
of all synthesized fly ash based hybrid materials recorded at
room temperature (Fig. 5). Photoluminescence study clearly
depicts that three main emission bands are present at 369,
410 and 468 nm. Photoluminescence intensity of samples
decreases from activated fly ash to Ba-N/FA attributes defects
in crystal lattice and vacancies of nanoparticles [37]. The
decrease in photoluminescence intensity proves the quenching
between fly ash with nitrogen, alkali metals and alkaline earth
metals.
Catalytic performance: The activities of catalyst were
investigated for Claisen-Schmidt condensation of substituted
4-chlorobenzaldehyde and acetophenone and the results are
given in Table-3. It shows that Ba-N/FA catalyst accelerates
the rate of reaction as compared to all other synthesized catalyst
in conventional as well as microwave irradiation method
(Scheme-I). The prepared Ba-N/FA catalyst was found to
possess significant basicity due to well synergy establishment
in between barium and nitrogen as compared to other prepared
hybrid catalysts, evident from reaction time and final yield.
The reaction time and final yield found to be less in comparison
with earlier reported work [24-26]. The application of this
synthesized material has the high activity, the simplicity of
preparation method, easily available raw materials, which can
be a benefit for its extensive application in organic synthesis
reaction. Synthesis of a series of chalcone derivatives were
TABLE-2
ELEMENTAL ANALYSIS BY XPS METHOD
Fly ash
Ba-N/FA
Region
Atomic (%)
37.91
32.20
12.15
10.08
6.24
Atomic (%)
10.00
48.60
26.93
8.06
C1s
O1s
Si2p
Al2p
Mg
–
Ca2p
Ba3d
N1s
1.42
–
–
–
5.36
1.05

2170 Ghoshir et al.
Asian J. Chem.
TABLE-4
CLAISEN-SCHMIDT CONDENSATION USING
Ba-FA/N CATALYZED BETWEEN SUBSTITUTED
ALDEHYDE AND SUBSTITUTED ACETOPHENONE
IN MICROWAVE IRRADIATION
Time
(min)
Yield
(%)
m.p.
(°C)
56
116
187
158
102
62
R1
R2
Ref.
Pure FA
H
4-Cl
4-OH
4-NO2
H
H
H
H
2
2
2
2
2
2
2
89
92
88
91
87
90
86
[[388]]
[[388]]
[[388]]
[[388]]
[[388]]
N-doped FA
Li-N/FA
H
4-Cl
4-OH
4-NO2
H
H
[38]
[38]
[[388]]
Na-N/FA
Mg-N/FA
Ca-N/FA
122
92
91
90
89
88
87
86
Sr-N/FA
Ba-N/FA
300
400
500
600
700
Wavelength (cm–1)
Fig. 5. Photoluminescence spectra of pure fly ash, N-doped fly ash, Li-N/FA,
NA-N/FA, Mg-N/FA, Ca-N/FA, Sr-N/FA and Ba-N/FA
TABLE-3
CATALYTIC ACTIVITY OF FLY ASH BASED
HYBRID CATALYST USED FOR CLAISEN-SCHMIDT
CONDENSATION BETWEEN 4-CHLOROBENZALDEHYDE
AND ACETOPHENONE
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
Weight of catalyst (g)
Conventional
Microwave
Catalyst
Fig. 6. Effect of BA-N/FA catalyst loading on the rate of reaction
Time (h)
Yield (%)
Trace
47
Time (min)
Yield (%)
Pure FA
N/FA
2.50
2.25
2.00
1.75
1.50
1.25
1.00
0.75
2
2
2
2
2
2
2
2
Trace
58
dehyde to form a β-hydroxy carbonyl ketone after dehydration
it produces chalcone by Claisen-Schmidt condensation shown
in Scheme-III.
Regeneration of catalyst:With the help of simple thermal
regeneration method the fly ash based hybrid catalyst was
regenerated and retained their catalytic activity which showed
the similar catalytic activity up to the fourth reaction cycle
giving the conversion of 4-chlorobenzaldehyde to chalcone
(92 %), indicates that basic sites are not deactivated in the regen-
erated catalyst as shown in Table-5.
Li-N/FA
Na-N/FA
Mg-N/FA
Ca-N/FA
Sr-N/FA
Ba-N/FA
55
66
74
78
80
86
66
73
81
84
85
92
prepared under the optimized conditions (Scheme-II), electron
donating as well as electron withdrawing group as substituents
on aldehyde and acetophenone in the presence of Ba-N/FA
catalyst using microwave irradiation. In this synthesis obtained
yields of chalcone derivatives, reaction time and yields as shown
in Table-4.
Effect of amount catalyst: Fig. 6 shows the catalytic
effect of Ba-N/FA in the synthesis of chalcone (Scheme-II)
by varying the catalyst quantity from 0.15 to 1.55 g. As the
catalyst quantity is increased from 0.1 to 0.75 g, the percentage
of yield is increased from 86 to 92 %, there is no significant
increase in the percentage of product by even after increasing
0.75 g of the catalyst.
Proposed mechanism: The catalytic activity of Ba-N/FA
is higher in comparison with other fly ash based hybrid catalysts.
It might be due to availability of maximum basic sites on the
surface, evident from XPS spectra, abstracts the proton from
acetophenone to form a carbanion which gives keto-enol equi-
librium. These enolate ion further attack on 4-chlorobenzal-
TABLE-5
REUSABILITY OF Ba-N/FA CATALYST ON CHALCONE
SYNTHESIS FROM 4-CHLOROBENZALDEHYDE AND
AETOPHENONE UNDER MICROWAVE IRRADIATION
Run
1
2
3
4
Yield (%)
92
91
90
88
Conclusion
In the present work, solid base fly ash hybrid materials
were prepared by co-doping of fly ash with alkali nitrate and
alkaline earth metals and nitrogen, separately by co-preci-
pitation method. The characterization of catalyst confirmed
that Ba-N/FA catalyst possess better crystallite size up 40 nm
hence higher surface area and higher basicity towards syn-
thesis of chalcone by Claisen-Schmidt condensation reaction

Vol. 31, No. 10 (2019)
Synthesis and Characterization of Co-Doped Fly Ash Catalyst for Chalcone Synthesis 2171
H
O
Basic sites
O
H
R2
O
Ba
O
O
C
H2
Ba
O
R2
H2C
OH
Si
-H2O
Si
Si
Fly ash support
O
R1
O
O
H2C
H
R2
R2
R1
O
H
O
O
OH
R2
-H2O
R2
R1
(Chalcone)
R1
Scheme-III: Proposed mechanism of synthesis of chalcone by Clasien-Schmidt condensation in presence of fly ash based hybrid catalyst
(Ba-N/FA) in microwave irradiation method
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reusable for further reaction purposes.
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