In: Other
Prepare cyclohexene from cyclohexanol. The cyclohexanol and phosphoric acid (catalyst) are placed in the distillation flask.
a) During the distillation process, why the receiving vessel be sitting in an ice bath? Why need to distil slowly?
Pour 10.6 ml Cyclohexanol into a 50 ml round bottom flask which
is having a small neck and cautiously add 85% Phosphoric acid (3
ml). Add 3 boiling chips and arrange for a distillation using a 10
ml graduated cylinder in an ice bath as a receiver. Heat the round
bottom flask slowly with a small flame. Stop the distillation when
white fumes appear in the round bottom flask, and about 10 ml of
distillate have been collected. Transfer the distillate to a 60 ml
separatory funnel ensuring that the stopcock of the separatory
flask is closed. The mixture will separate into two layers.
Run off the lower layer into a conical flask and set this aside.
Add 10 ml water to the liquid in the separatory funnel and shake to
allow thorough mixing of the liquids. Allow the layers to separate.
Cyclohexene will separate out from the water. Run off the aqueous
layer and collect the Cyclohexene.
The receiving vessel is placed in an ice bath because if it is not placed in it, the product will evaporate resulting in lower yield and increased stench in the surroundings.
The completion of reaction takes time due to the formation of carbo cation intermediates. So, tthe distillation process must be done slowly.