1. Place 10.0mL cyclohexanol in a 250 mL Erlenmeyer flask and then add 25mL of g
ID: 479422 • Letter: 1
Question
1. Place 10.0mL cyclohexanol in a 250 mL Erlenmeyer flask and then add 25mL of glacial acetic acid. Place the flask in an ice 2. Using an addition funnel, add 75mL of a 5%NaOCI solution (laundry bleach) dropwise, with occasional stirring, at such a rate that the temperature is kept between 30 and 35 C After addition of the first 75mL. swirl the reaction well, returnitto the ice bath and add an additional 75mL of 5% NaOCI dropwise without letting the temperature get above 35 C 3. Test the reaction mixture with po iodide-starch paper. If a positive reaction not obtained, add 1-5 mL more of the NaOCI solution until a positive reaction Let the reaction mixture stand at room temperature for 15 minutes. Then add saturated sodium bisulfite solution until the mixture gives a negative KI-starch test While waiting, obtain the IR of the cyclohexanol starting material Transfer the reaction mixture to a 250mL round bottom flask. Distil the mixture until the distillate appears free of droplets (75 100 mL) Collect the distillate in an Erlenmeyer flask. 5. Pour the distillate into a large beaker (to contain the foaming in the next step) and set it on a magnetic stimer Add a magnetic stir bar. To free the distillate of acetic acid, add sodium carbonate carefully, with stirring. until foaming ceases. 6. Add 8g of sodium chloride (dissolved in a minimum amount of water) to further salt out the cyclohexanone. Decant the mixture into a separatory funnel and separate the layers. Place the cyclohexanone into a small Erlenmeyer flask. Return the aqueous layer to the separatory funnel and extract it of methylene chloride. Add the with 5mL methylene chloride extract to the cyclohexanone obtained in the first 7, Dry the cyclohexanone layer over anhydrous magnesium sulfate. Pour the solution through a cotton plug into a tared 25mL round bottom fiask. Rotovap the solution to remove methylene chioride (waste container). Reweigh the flask to determine the yield of cyclohexanone.Explanation / Answer
Salting out (also known as antisolvent crystallization, precipitation crystallization, or drowning out) is an effect based on the electrolyte-nonelectrolyte interaction, in which the non-electrolyte could be less soluble at high salt concentrations. It is used as method of separating compounds. The salt concentration needed for the compound to precipitate out of the solution differs from compound to compound. This process is also used to concentrate dilute solutions of proteins. Dialysis can be used to remove the salt if needed.
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