First the glassware apparatus for the reaction was set up. 3. 861-grams of isoborneol, 2. 21-mL of glacial acetic acid, and 4. 39-mL of 6% NaOCl solution were mixed in a 125-mL Erlenmeyer flask. Another 35-mL of 6% NaOCl solution was added to a separatory funnel and supported over the flask. The NaOCl in the sep funnel was slowly added into the Erlenmeyer flask with vigorous swirling, approximately 2-mL every 30 seconds until all the NaOCl from the sep funnel had been added. The temperature of the reaction mixture was closely monitored using a thermometer to make sure the temperature did not rise above 50?C.
After the addition completed, a watch glass was placed over the reaction flask and the flask was allowed to stir for 30 minutes. The reaction mixture was tested for excess hypochlorite every 5 minutes. After the 30 minutes the reaction mixture was tested again and this time it tested positive for hypochlorite so few milliliters of sodium bisulfite were added to give a negative test. Separation: The reaction mixture was cooled to 5?C in an ice bath. Next, the crude product was collected by vacuum filtration, washing it on the filter with two portions of cold water.
The crude product was dried at room temperature and then transferred to a pre-weighted plastic vial and left to dry on the desiccator for a period of one week. Part 2: Purification and Analysis The crude product was weighed and a small portion of it was sent for a crude infrared analysis. A sublimation apparatus was set up and the rest of the crude product was purified by sublimation. The side arm test tube was packed with an inch of the crude product and the product was heated using a Bunsen burner. The crystals that formed on the cold finger were collected and sent in for a pure infrared analysis.