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Practical Synthetic Techniques
Practical Synthetic Techniques
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Note: Some of the diagrams may be slightly different from whatever you’ve been taught, if that’s the case just stick to
what you usually draw. ☺thymolphthalein
Mixing
● Lots of organic chemistry involves immiscible liquids and you would have to shake/stir
the reaction mixture for a reaction to occur.
● Shaking is normally practicable in stoppered flasks in reactions that do NOT build up
pressure.
● Stirring can be done using a magnetic stirrer, if the reaction does not require heating.
Otherwise, a mechanical stirrer can also be used.
● It looks like this. Basically a flask kept on top of the device. You are not required to label
the parts or know how it works.
Heat Under Reflux
● Organic reactions are slow as they have high activation energies. Hence, heating is
required. Organic mixtures are also usually volatile to some extent, and heating the
mixture causes them to escape. This can be a fire/health hazard and may lead to a
decrease in yield. In order to prevent loss, heating is carried out under reflux.
● This technique is also used to supply energy to reactions over a long period of time.
● For safety: Use steam bath/electric heating mantle
● You must have: an open top, correct water in/out on the condenser, a pear shaped flask
and a source of heat. I’ve never seen antibumping granules being needed to get the
mark.
● You must show the tap in your diagram and label the layers correctly.
Büchner Funnel Suction Filtration
● Büchner funnels are used in filtrations that are carried out under reduced pressure. This
technique is used to prevent mechanical losses of the organic materials.
● How it works: Reduction of pressure below a perforated plate supporting the filter paper
causes the atmospheric pressure to drive the liquid through.
● This speeds up the process and dries the solid as most of the liquid is forced through.
● The apparatus should be set up like this. ALL THOSE LABELS ARE NOT NECESSARY.
The most important labels would be the vaccum tap, the funnel and flask, and the filter
paper. Note the specific shape of the Büchner funnel which is different from an ordinary
funnel.
Re‑crystallization
1. Dissolve in minimum amount of hot solvent . A suitable solvent is one in which the
solubility of the given solid increases WITH temperature.
2. Filter the solution in hot condition using preheated funnel with fluted filter paper. This
removes insoluble impurities in the mixture (cork, filter paper, other random stuff that
somehow got into your mixture idk)
3. Cool the filtrate in ice until crystals appear .
4. Filter the crystals via suction filtration/reduced pressure using a Büchner funnel. This
removes soluble impurities in the derivative.
5. Wash the crystals with a little amount of cold solvent.
6. Dry the crystals by pressing between two wads of filter paper and then by indirect heat
reflected from Bunsen burner.
7. Determine melting point and compare with Data Booklet/literature to check for purity!
Note: You may have been taught this slightly differently such as ‘indirect heat from oven’ instead
of Bunsen burner. If so just use what you’ve been taught as long as the mark schemes accept it.
Melting Point Determination
● Purity of a solid is usually determined by the melting point.
● The process is pretty simple:
1. Crush a small sample of the solid on a clean porous tile (which would absorb traces of
solvent remaining) and push the crushed solid into a capillary tube. If the solid gets stuck
at the top, gently tap the tube to dislodge the solid.
2. Attach thermometer to capillary tube using a rubber band and place in the oil bath. The
temperature must be raised very slowly as it gets nearer to the melting point.
3. Pure solids have a sharp melting point, and the sample will NOT appear to melt over a
‘temperature range’. This can be used for identification of the solid.
Note: As far as I know, you can use a boiling tube or a beaker for your oil/water bath. Or place
capillary tube in a boiling tube which is then placed in the bath. Just go with whatever you learnt
or is in your textbook. The setup should be something like this:
● Label the capillary tube, thermometer, water/oil, and the solid to be tested.
Distillation/Simple Distillation/Normal Distillation a.k.a not Fractional
Distillation ☺
● Distillation is used to separate organic liquids from solids or to separate liquids which
differ in boiling temperature considerably.
● On distillation, liquid with a lower boiling point distills off first and gets collected as liquid
in the flask at its boiling temperature.
● Label the correct water in/out and heat, thermometer should be aligned with where the
condenser tube starts.
Fractional Distillation
● Generally used to separate liquids which differ in boiling point temperatures slightly and
is more efficient.
● Process depends on the fact that the vapour above a mixture of liquids is richer in the
more volatile component (low boiling temperature).
● Only ideal solutions ( mixtures which have the same intermolecular forces as in pure
liquids of the components* ) such as hexane/heptane, benzene/methyl benzene,
chloromethylbenzene/benzene, and ethanol/methanol.
● Fractionating column has a large surface area on which the ascending vapour and
descending liquid comes into contact. A mixture rich in the more volatile component
distills over at the top of the column, where the temperature measures its boiling
temperature.
● As distillation continues, temperature rises towards the boiling point of the next volatile
component. Components are distilled over at the top of the column at their boiling points.
Distillation is a good way to measure boiling temperature.
Steam Distillation
● Steam distillation works on the principle that immiscible substances when mixed together
can lower the boiling point of each other.
● Certain compounds, such as many organic compounds which have high boiling points
can be distilled using this technique. It is very useful for extracting molecules with a high
boiling point which might thermally decompose under normal conditions.
● So there’s a lot of differentish diagrams for this. Stick with the one in textbooks/what
you’ve been taught. But there should be water being heated to release steam, a mixture
which is being steam distilled, and a condenser.
Solvent extraction
Just adding this here, copy pasted as an answer I gave to someone. Will write in point form if I
have time.
“ It's usually used when you have an organic product as an aqueous solution i.e. mixed with
water. To extract the organic product, you want to mix it with something that is immiscible with
water BUT is a better solvent for the organic product than water.
So for example if you have a solution of B in water you mix it with an organic solvent such as
hexane by shaking the solutions together. As B is more soluble in hexane, it will dissolve in that
layer and not in the water layer. You can use a separating funnel to mix the two and let it settle,
and collect the hexane layer.
After this you can use another process to obtain the organic compound, but that is not part of
the technique of solvent extraction itself. Generally, you'd use distillation, I guess.
That's why ethoxyethane is commonly used for solvent extraction. It is immiscible in water, a
good organic solvent and has a low boiling point.
Thin Layer Chromatography
Draw a pencil line near the bottom of the plate. Place a spot of the mixture you want to test and
place spots of known amino acids on the line.
Put some suitable solvent into a large beaker, and stand the plate inside the solvent. It is
important that the solvent level is below the line with the spot on it.
Cover the beaker so that solvent does not evaporate.
Leave the plate long enough for spot to separate, remove the plate and mark the position of the
solvent front. The spots will still be invisible.
Spray the plate with ninhydrin and heat in an oven. Purple spots should appear and you can
compare the spots with how far the reference amino acid spots have moved.