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Introduction
An apparatus for simple distillation was set up. 100 ml round-bottom flask and 50
ml round-bottom flask was used as the distilling flask and receiving flask. An ice
bath was placed around the receiver to lessen the loss of product by evaporation.
Then, an empty 100 ml round-bottom flask was weighed. 7.5 ml of
4-methylcyclohexanol was placed using graduated pipets and the flask was
reweighed again to get the mass of alcohol. 2.0 ml of 85% phosphoric acid and 30
drops of concentrated H2SO4 along 2 boiling chips was added in the distillation
flask and mix thoroughly. The mixture was heated with a heating mantle and
distilled slowly with maintain the distillation temperature below 100℃.
Distillation was continued untill only 0.5-0.6 ml of residue remains in the flask or
the mixture began to smoke or bump. Next, the distillate was mixed with 3ml of
saturated NaCl and the mixture was transfered into a test tube. The test tube was
closed with the cork tightly and the layers was mixed by swirling and shaking.
This step was repeated to allow the layers to separate. The bottom aqueous layer
was drawn off with a Pasteur pipet and discarded. The crude of
4-methylcyclohexene was transfered using pasteur pipet to an Erlenmeyer flask. A
small amount of anhydrous Na2SO4 was added and a stopper was placed. The
liquid was dried for at least 15 minutes while gentle swirling. The simple
distillation was cleaned,dried and reassambled with acetone during drying interval.
A receiver of 50 ml round-bottom flask was weighed and transfered the dried
cyclohexene with pasteur pipet into 100 ml round-bottom flask. 2 boiling chips
was added and distilled and repeated the step as above for distillation process.after
that,the flask was reweighed and calculate the percentage yield of
4-methylcyclohexene.