1. General

At this point in the quarter, it would be very advisable to review your infrared spectroscopy and NMR spectroscopy notes from lecture. You are expected to have mastered these topics by the time the final exam comes around (in about three weeks). You will need to memorize the most important numbers and trends for the exam because there will be no tables provided!

2. Experiment

Safety notes:

1. The glassware can be very hot when removing it from the microwave. Use a paper towel when removing the Erlenmeyer flask.

2. Only the TA is allowed to operate the microwave.

3. Do not look directly into the UV-lamp. The UV-light will damage your eyes.

a. It is very important the reactants and the catalyst are well mixed before placing the mixture in the microwave.

b. The reaction mixture has to be well insulated after removing it from the microwave. This will guarantee that the reaction continues afterwards.

c. If the compound does not crystallize upon cooling, the solution can be reheated. A few drops of water are added to the solution (until it is a little cloudy) before the mixture is allowed to cool down.

d. The GC/MS sample (2 mg/mL in ethyl acetate) cannot contain any solids.


3. Things to think about

a. What would happen if the student would use a large excess of ethyl acetoacetate?
b. Where do you see the advantage of using Amberlyst A15 compared to p-toluenesulfonic acid?
c. What would the student observe in the fluorescence test if the pH-value of the solution was too high (pH>11)?
d. What would change in the fluorescence test if the student uses a shorter wavelength for the excitation?