Measure 0.5 ml of 2-ethyl-1,3-hexanediol into a tared 10 mL round-bottom flask.

Question

Measure 0.5 ml of 2-ethyl-1,3-hexanediol into a tared 10 mL round-bottom flask. Reweigh the flask to determine the mass of diol added. Clamp the flask to a ring stand and add 3 ml of glacial acetic acid and a magnetic stir bar. Lower the flask into an ice bath in a small beaker (50-ml or 100-mL) and begin stirring the mixture. Watch out! Adding NaOcI Using a clamp, place a thermometer in the flask so that it measures produces heat and the product is the temperature of the solution while still allowing the stir bar to heat sensitive. Add NaoC rotate freely. dropwise (one drop at a time). The rate of dropping can be adjusted While stirring the mixture, slowly add 3 mL of 5% aqueous ! sodium hypochlorite (bleach) dropwise. Monitor the temperaturedsed o closely, and do not allow it to rise above 30 °C. Once the addition is complete, remove the ice bath and continue stirring at room temperature for 1 hour. reaction solution. For complete reaction it is necessary to have an excess of sodium hypochlorite. Every 15 minutes test the solution by transferring a drop of the reaction mixture to a starch/iodide test strip. If the paper turns blue or black within a few seconds there is an excess of hypochlorite. If not, add 0.5 mL of sodium hypochlorite solution and repeat the test in five minutes. 5-10 minutes before the reaction is complete prepare an ice-brine bath with 10 mL of brine and 10 ml of ice. After the reaction is complete, pour the re action mixture into the ice-brine bath. Transfer to a 50 ml centrifuge tube and extract with three 10 mL portions of diethyl ether. Cap the centrifuge tube and rock il back and forth to mix the layers, remembering to vent carefully every 15- 30 seconds. Combine the ether extracts and wash with two 5 ml portions of saturated sodium carbonate then two 5 mL portions of 5% aqueous sodium hydroxide. Take a small piece of pH paper, wet it with a drop of DI water, and touch the moistened paper to the surface of the ether layer. If it is not basic, wash again with an additional portion of 5% sodium hydroxide solution. Dry the ether solution over a magnesium sulfate. Decant or gravity filter into a tared 50 mL round bottom flask and remove the ether by rotary evaporation. The product will be a liquid, and so it may difficult to determine when all of the ether has evaporated. Once the bubbling of ether stops, leave it on the rotovap for an additional 2-3 minutes to ensure any remaining traces of ether evaporate. Determine the % yield, and collect the IR spectrum. mass an

Explanation / Answer

Source of Error in the Oxidation of 2-ethyl-1,3-hexanediol are:-

- Addition NaOCl (Bleach) in a proper manner) otherwise it produces heat .i.e. Exothermic reaction

- NaOCl .i.e. sodium hypochlorite bleach is keep on dripping so openning at the separatory funnel prevents vacuum formation.

- Three products were reported carefully

- Atom economy calculation should be proper

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