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Lab Report CHM 457 Exp 2

This laboratory report describes an experiment to prepare 4-methylcyclohexene through the dehydration of 4-methylcyclohexanol. Key steps included assembling distillation apparatus and heating a mixture of the starting material, phosphoric acid, and sulfuric acid to distill off the product. Tests with bromine and potassium permanganate solutions confirmed the presence of an unsaturated bond in the isolated product.

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Irfan Azahar
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230 views

Lab Report CHM 457 Exp 2

This laboratory report describes an experiment to prepare 4-methylcyclohexene through the dehydration of 4-methylcyclohexanol. Key steps included assembling distillation apparatus and heating a mixture of the starting material, phosphoric acid, and sulfuric acid to distill off the product. Tests with bromine and potassium permanganate solutions confirmed the presence of an unsaturated bond in the isolated product.

Uploaded by

Irfan Azahar
Copyright
© © All Rights Reserved
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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LABORATORY REPORT

FUNDAMENTAL ORGANIC CHEMISTRY


(CHM 457)

EXPERIMENT 2: preparation of 4-methylcyclohexene from


dehydration of 4-methylcyclohexanol

NAME OF STUDENT : 1) Irfan Nurhadi bin Azahar (2020819572)


2) Farisha Husna Binti Azman (2020897392)
3) Nadiatulmaisarah Ali (2020853166)

PROGRAMME/ GROUP :AS2222A1


DATE OF EXPERIMENT :  21/4/2021

DATE OF REPORT SUBMISSION:  28/4/21


NAME OF LECTURER : DR ROHAIZA SAAT

CHECMICALS & APPARATUS


CHEMICALS: 4-methylcyclohexanol, 85% phosphoric acid, concentrated sulfuric acid,
saturated chloride solution, granular anhydrous sodium sulfate, bromine test reagent,
potassium permanganate test reagent.
APPARATUS; 50ml round bottom flask, 25ml round bottom flask, erlenmeyer flask,
glass stirring rod, Pasteur pipette, boiling stone, distillation apparatus, ice-water bath,
heating mantle, weighing balance.

PROCEDURE

 ASSEMBLY APPARATUS.
7.5ml of 4-mthylcyclohexanol was placed in a tared 50ml round bottom flask and
reweigh. 2.0ml 85% of phosphoric acid and 30 drops of concentrated sulfuric acid
was added in a flask. The mixture was stirred by using rod and boiling stone was
added in it. Distillation apparatus was assembled while 25ml round bottom flask
acted as receiver. The receiving flask was immersed in an ice-water bath.

 DEHYDRATION
Cooling water start circulated in the condenser and the product was collected in the
receiver after the mixture heated by using heating mantle until distilled. The heating
was regulated in order distillation to complete in 30 minutes.

 ISOLATION AND DRYING OF THE PRODUCT


The distillate was transferred to a centrifuge tube with the aid of 1 or 2 ml of
saturated sodium chloride solution. Bottom aqueous layer was removed by using
Pasteur pipette and the remaining organic layer was transferred with another dry
Pasteur pipette in erlenmeyer flask that contain a small amount of granular anhydrous
sodium sulfate. To remove the last traces of water the flask was set aside around 10-
15 minutes by place the stopper on the flask. Drying process was done by wash and
dry the distillation apparatus with small amount of acetone and air stream.

 DISTILLATION
The dried liquid was transferred as much as possible into the round bottom flask.
Distillation apparatus was set up as before and using preweighed 25ml receiving
flask after boiling stone added in flask. The material that boils over range 100-105℃
was collected after distilling the 4-methycyclohexene by using heating mantle.
Observation of boiling point was recorded in notebook. The receiving flask was
reweighed and percentage of yield of 4-methylcyclohexene was calculated.

 UNSATURATION TEST
Two small test tube was added 4 drops of 4-mthycyclohexene for each of it by doing
the same thing to another of two small test tube by labelling group A and B. the
solution of bromine in carbon tetrachloride or methylene chloride was added drop by
drop to the content test tube in one of the test tube from each group until the red
colour no longer discharged. The result was recorded included the number of drop
too. The other remaining test tube was performing the same method by using solution
of potassium permanganate after add 0.3ml of 1,2-dimethoxyethane. The result was
recorded.

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