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The microwave chemistry is also called as Green Chemistry.
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Define Scale up process, need of Scale up technique, Stages of scale up process Bench\lab scale, pilot plant, large scale up technique, validation of large scale up process
Process chemistry AS PER PCI SYLLABUS FOR M.PHARMShikha Popali
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Presented by Shikha Popali and Harshpal singh Wahi students from Gurunanak college of pharmacy, Nagpur in Department of pharmaceutical Chemistry. The explained topic is seful for every chemistry student and for others too
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MERITS OF MICROWAVE ASSISTED REACTIONS
DEMERITS OF MICROWAVE ASSISTED REACTIONS
MECHANISM OF MICROWAVE HEATING
EFFECTS OF SOLVENTS IN MICROWAVE ASSISTED SYNTHESIS
MICROWAVE VERSUS CONVENTIONAL SYNTHESIS
MICROWAVE INSTRUMENTATION
VARIOUS TYPES OF MICROWAVE ASSISTED ORGANIC REACTIONS
APPLICATIONS OF MICROWAVE ASSISTED REACTIONS
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microvave assisted reaction.pptx
1. Microwave assisted reactions
Presented by
Dhanashree R. Kavhale
M. Pharm. (Pharmaceutical Chemistry) Sem- II
Department of Pharmaceutical Sciences,
Rashtrasant Tukadoji Maharaj Nagpur University, Nagpur - 440033
3. What are microwaves?
Microwave is a form of electromagnetic radiation with wavelength ranging
from about one meter to one millimeter corresponding to frequencies between
300 MHz and 300 GHz respectively.
It uses the EMR that pass through material and causes the oscillation of
molecules which produces heat.
3
4. Microwave Irradiation
Microwaves act as high frequency electric fields and will generally heat any
material containing mobile electric charges, such as polar molecules in a
solvent or conducting ions in a solid.
MW energy is non ionizing and thus does not change the molecular
structure of the compound, it only provides thermal activation.
Microwave irradiation provide the enhanced reaction rate or speed to the
chemical reaction.
Along with the formation of variety of carbon heteroatom bonds.
4
5. Conventional heating v/s Microwave radiation
technique
• involves the use of a furnace or oil bath, which
heats the walls of the reactor by convection or
conduction.
• The core of the sample takes much longer to
achieve the target temperature.
Conventional
heating
• microwave radiation acting as internal heat
source.
• Microwave absorption is able to heat the target
compounds without heating the entire furnace or
oil bath.
Microwave
technique
5
6. Microwave assisted reactions
Microwave irradiation has gained popularity as a powerful tool for rapid and
efficient synthesis of a variety of compounds because of selective absorption of
microwave energy by molecules.
This phenomenon is dependent on the ability of a specific material to absorb
microwave energy and convert it into heat.
Microwave passes through material and causes oscillation of molecule which
produces heat.
Microwave heating produces heat in the entire material in the same rate and at
the same time at a high speed and at a high rate of reaction.
Microwave heating is the best process due to the microwave couple directly with
the molecule that are present in the reaction mixture, leading to fast rise in
temperature, faster reaction and cleaner chemistry.
6
7. The microwave chemistry is also called as Green Chemistry because it does not
produce any hazardous material like gas, fumes, etc.
Microwave heating rate can be depending upon dielectric properties of material.
Dielectric properties describe the ability of a material to absorb, transmit and
reflect electromagnetic energy.
Less polar and
highly
crystalline
materials are
poor absorber.
Compound
with high
dielectric
constant tends
to absorb mw
energy.
Magnitude of
energy
transfer α
dielectric
properties of
molecules.
7
8. Mechanisms of microwave heating
All the materials are not susceptible to microwave heating as response of
various materials to microwave radiation is diverse.
Microwave absorbing materials (e.g. water) are of utmost important for
microwave chemistry.
There are three main different mechanisms are involved for their heating
namely:
1. Dipolar polarization
2. Conduction mechanism
3. Interfacial polarization.
8
9. Continue…
Dipolar polarization
For a substance to be able to generate heat when irradiated with microwaves it
must be a dipole, i.e. its molecular structure must be partly negatively and partly
positively charged.
Since the microwave field is oscillating, the dipoles in the field align to the
oscillating field.
This alignment causes rotation, which results in friction and ultimately in heat
energy.
9
10. Ionic conduction
During ionic conduction, dissolved (completely) charged particles (usually ions)
oscillate back and forth under the influence of microwave irradiation.
This oscillation causes collisions of the charged particles with neighboring
molecules or atoms, which are ultimately responsible for creating heat energy.
Continue… 10
11. Interfacial polarization
The interfacial polarization method can be considered as a combination of both
the conduction and dipolar polarization mechanisms.
It is important for heating systems that comprise a conducting material dispersed
in a non-conducting material.
Continue… 11
12. Higher temperature can be obtained.
Faster reactions, lesser by products, pure compounds.
Better yield and higher purity.
Absolute control over reaction parameters.
Uniform and selective heating.
Energy efficient, rapid energy transfer.
Easy access to high pressure performance.
Does things that can't be done conventionally.
Rapid synthesis results in lesser evaporation of solvents.
Merits of microwave assisted reactions 12
13. Continue…
Green synthesis
- Possibility of convenient solvent superheating.
- Excellent parameter control.
- Access to automated setups and parallel synthesis.
- Possibility of stirring.
- Continuous power output.
13
14. Demerits of microwave assisted reactions
sudden increase in temperature may led to the distortion of molecules.
Reactions are very vigorous and which may be hazardous.
Heat force control is difficult Water evaporation.
Closed container is dangerous because it could be burst.
Short reaction period, so care must be taken during the process.
Microwave reactors are expensive so care must be taken during their use.
Many other things like, temperature sensitive reactions, reactions involving
bumping of material, reaction which effervescences and color reaction are not be
done in microwave reactor.
14
15. Superheating effects of microwave
Temperature of solvent above its normal boiling point due to heating by
microwave is called superheating.
Superheating is due to:
1. direct interaction of microwaves with molecules of entire solvent causing
sudden rise in temperature.
2. nucleation sites-present on container wall prevents vaporization of energy
to top surface of solvent.
If 1lit og water is superheated by only 1℃, it can produce about 3 lit of
steam.
15
16. Increased reaction rate
Microwave heating depends on two major factors:
factor "A" which describe thermomolecular mobility and depends upon the
frequency of vibrations of the molecule at reaction interface.
The other reason is the alteration in the exponential factor by affecting the free
energy of activation of delta G4.
We know that with every 10℃ rise in temperature the rate of reaction become
double.
For a reaction to be completed it takes 80 min in conventional system but if the
same reaction takes place in microwave irradiation it takes only 10 min this
shows that in microwave irradiation the rate of reaction speeds up.
16
17. References:
1. Nüchter M, Ondruschka B, Bonrath W, Gum A. Microwave assisted
synthesis–a critical technology overview. Green chemistry. 2004;6(3):128-41.
2. Caddick S. Microwave assisted organic reactions. Tetrahedron. 1995 Sep
18;51(38):10403-32.
3. Grewal AS, Kumar K, Redhu S, Bhardwaj S. Microwave assisted synthesis: a
green chemistry approach. International Research Journal of Pharmaceutical
and Applied Sciences. 2013 Oct 31;3(5):278-85.
4. Yadav AR, Mohite SK, Magdum CS. Comparative study of conventional and
microwave assisted synthesis of some organic reactions. Asian Journal of
Pharmaceutical Research. 2020;10(3):217-20.
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