Experiment 8: preparation of cyclohexene from cyclohexanol
Chemicals: Cyclohexanol 85 % phosphoric acid Sodium chloride
solid 10% sodium carbonate solution Anyhydrous magnesium sulphate
Boiling chips Ice cubes KMno4 solutionApparatus : Thermometer Still
head Condenser Round bottom flask Receiving flask Rubber hoses
Conical flask Adapters Retort stand Gravity funnel Water bath
Saparatory funnel and stopper Test tube
Procedure1. Simple distillation was set up2. 10 -15 mL of 85 %
phosphoric acid in a round bottom flask3. 20 mL of cyclohexanol was
added with a few boiling chips4. The reaction mixture was
distilled5. The receiving flask was immersed up its neck in an ice
bath to avoid loss of any product6. The distillation flask was
immersed carefully so that a steady distillation rate obtained7.
The temperature was controlled in order not to exceed 103 0C.The
heating process was stopped when the temperature exceed 103oC.8.
The distillate was saturated by adding solid sodium chloride
portion with swirling.9. 10 % of sodium carbonate was being added
to neutralized the adicic10. The mixture was transferred to a
separatory funnel and an aqueous layes was drained off11. The
organic layer was poured into a conical flask and being dried with
anhydrous magnesium sulphate12. The product was filtered into round
bottom flask via gravity filtration13. The dried cyclohexene was
redistilled14. The boiling point was recorded and the volume of the
product was measured15. The product was tested with a few drops of
KMno4
