Last updated Fri, Oct 25, 2002

1. General

Review the following topics: IR spectroscopy

Don't forget to start writing your formal report. By now, you should be able to write an introduction and the experimental part for first couple of parts.

2. Experiment

The potassium carbonate has to dissolve first before you can start adding the aldehyde. This is very important.

If you didn't get any aldehyde from your reaction, the TA will supply some for you. In this case, downscale the reaction using 1.0 g of the aldehyde.

Make sure that you set the temperature to a gentle reflux and don't forget to stir it.

A reflux period of 45 minutes is usually sufficient in order to complete the reaction.

During the drying step, make sure that you follow the washing procedure correctly: first water, then saturated sodium chloride solution and last the drying agent in the organic layer only (try to remove the aqueous layer as good as possible).

For procedure how to use the polarimeter see link.

3. Thing to think about

a. Why do you add water to the reaction mixture before you allow it to cool down?

b. How many signals do you expect to see in the 13C-NMR spectrum of the ligand?

c. How does the polarimetric measurement help to establish the absolute configuration and purity of the ligand?