Time can be very valuable if it is used to wrap up one project and make preparations for the next one. Today, my group tested our individual cyclohexanone samples from the oxidation experiment, performed the next portion of the Baeyer-Villiger oxidation, and set up the apparatus for a Grignard reaction.
From the IR spectrum of my cyclohexanone sample, the OH peak has significantly reduced from the last experimental run. Since the GC suggests that no more cyclohexanol remains in the solution, we suspect that there is still water in the system or that some the cyclohexanone has been converting to its enol form. We will extract the liquid from the vial containing drying agent prior to our next run of the Baeyer-Villiger reaction.
The workup following the Baeyer-Villiger reflux involved transferring the contents of the reaction flask to an Erlenmeyer flask, using 30 mL of dichloromethane to make a qualitative transfer. After that, the solution was left to stir with 30 mL of water. Adding 0.15 g of sodium bisulfite and 10 mL of 10% sodium bicarbonate solution formed two separate layers in the reaction mixture after vigorous fizzing. We will complete the reaction tomorrow, once the mixture has been stirred through the night.
The apparatus we set up is, in one word, AWESOME, and I will post a picture of it tomorrow...brace yourselves....
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