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Synthesis of Benzil EXP 4

The document summarizes the synthesis of benzil from crude benzoin using nitric acid. Crude benzoin is oxidized with nitric acid in a round-bottomed flask with occasional shaking for 1.5 hours. The reaction mixture is then poured into cold water and filtered to isolate the crude benzil product. The crude benzil is recrystallized from ethanol and its melting point is measured to determine purity by comparing to the theoretical melting point. Safety precautions are outlined for handling nitric acid, crude benzoin, and ethanol during the experiment.

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287 views4 pages

Synthesis of Benzil EXP 4

The document summarizes the synthesis of benzil from crude benzoin using nitric acid. Crude benzoin is oxidized with nitric acid in a round-bottomed flask with occasional shaking for 1.5 hours. The reaction mixture is then poured into cold water and filtered to isolate the crude benzil product. The crude benzil is recrystallized from ethanol and its melting point is measured to determine purity by comparing to the theoretical melting point. Safety precautions are outlined for handling nitric acid, crude benzoin, and ethanol during the experiment.

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Gobe Jam
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SYNTHESIS OF BENZIL

GOBE JAM CHEM 305

PRE LAB
INTRODUCTION
Benzil is an organic with an IUPAC name diphenylethane-1,2-dione of the chemical formulae
(C6H5CO)2. It is a yellow solid that can be decomposed into free radical species by the
ultraviolet radiation. In the synthesis of the compound, benzoin is oxidised into in the presence
of the concentrated nitric acid. The synthesis of the compound is simply the continuation of the
tetraphenyl cyclopentadienone. During the synthesis of Benzil the heated mixture is cooled in
cold water and then filtered to separate the solid from the liquid part before filtration. The
melting point of the product is then measured and later compared to the theorical melting point
as one of the ways to determine its purity ( Depreux et al,2008). The reaction mechanism of this
synthesis is demonstrated in the figure below:

It is important to note that because sulphuric acid is not present during the process, the aromatic
ring is not being nitrified. Benzil can be classified as a selective inhibitor of carboxylesterases
enzymes, proteins involved in the metabolism of esterified medicines and xenobiotics, according
to (Jadhav et al., 2017). The crucial stages I employed throughout the experiment were
crystallization and recrystallization, and crystallization is frequently used to purify solid
compounds. The purified, solid crystal is typically kept intact in the solution while the two
methods typically enable impurities to stay dissolved in a solvent.

OBJECTIVE
 The main objective of this experiment is to synthesis Benzil from the crude benzoin in an
acidic environment, obtain its percentage yield and melting point to confirm its purity.

MATERIALS
1. REAGENTS AND APPARATUS USED
 Crude benzoin
 ethanol
 Nitic acid
 Distilled water
 100ml round bottomed flask
 Drying oven
 50ml beaker
 Stirring rod
 Pump
PROCEDURE
In the beginning of the experiment, 2.000 g of the crude of benzoin was measured with an
analytical balance and added into a 100ml round bottomed flask with 10ml of nitic acid. The
mixture was heated in a water bath with occasional shaking until the evolution of oxides of
nitrogen had ceased and that was for about 1.5 hours. The reaction mixture was poured into 30ml
cold water in a beaker and stirred well until the oil had crystallized completely well as a yellow
solid. The crude benzyl was then filtered at the pump and washed thoroughly with water to
remove the nitric acid. The solid was then recrystallized from the ethanol and then the melting
point determined after removing from the drying oven.

Molecule structure
I. Crude benzoin

II. Nitric Acid

III. Crude benzyl ethanol

Safety precaution
 When handling nitric acid in the laboratory, it’s recommended to wear chemical safety
glasses, a face shield for splash protection, gloves, and an approved vapor respirator if
adequate ventilation is not available. As an added safety precaution, eyewash stations and
washing facilities should be easily accessible.

 When working with crude benzoin avoid inhalation & direct contact with skin & eyes of
crude benzoin and do not discharge into drains, water courses or onto the ground.

 Ethanol is a highly flammable liquid and vapor. Causes serious eye irritation. May cause
genetic defects. Therefore, it is advisable to avoid contact and always wear safety gloves
and goggle.

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