2.08 grams of cyclohexanol and 0.5 mL of 85% phosphoric acid were added to a micro round bottom flask. The solution was heated and boiled in a fractional distillation apparatus until about 10% volume of the solution remained. The distillation started at a temperature of approximately 70°C and reached a temperature of approximately 72°C at the completion of the distillation. After the distillation the solution of water and cyclohexene distillate was transferred into a reaction tube. Another 1mL of water was added to the tube and backwashed. The lower layer of the tube was removed into a waste beaker. 1 mL of sodium hydroxide was then used to backwash the organic layer. The bottom layer was removed to waste and then 1 mL of brine was used to backwash the organic layer again. The bottom layer was removed to waste. The solution was then dried with CaCl2 and transferred into a tared vial to yield the cyclohexene product (0.729 grams, 42.63% yield). The product was verified by performing a test by adding a solution of 3% bromine in dichloromethane (3 drops) into 0.5 mL of the cyclohexene product and 0.5 mL of cyclohexane. Color changes and precipitate formations were noted. Then another test was performed by adding 3 drops of potassium permanganate to 0.3 ml of cyclohexene and 0.3 mL of cyclohexane. Color changes and formation of precipitates were noted again. Finally, GC and IR tests were performed to assess the purity of the product.
Recent comments