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Unformatted text preview: It must be connected to a Variac to regulate the voltage. Always inspect the bottom of an oil bath for water droplets. Water in an oil bath may explosively vaporize and spray hot oil when the bath is heated near or above 100 C. Use a silicone oil bath, as other oils may break down at this temperature (210 C). Preheat the oil bath to a stable temperature beforehand. This may take some time, so start heating the oil bath first, then mix the reagents. 3. Characterization and Report Determine the yield of product both, crude and after each purification step. List the column conditions used and the R f values of estrone and any major impurities in the crude reaction mixture. Characterize the recrystallized estrone by IR, 1 H and 13 C NMR, and melting point. Tabulate and assign the spectral data. Find a literature reference for the synthesis of racemic estrone. Compare your characterization data with the literature values....
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This note was uploaded on 01/03/2012 for the course CH 5a taught by Professor List during the Fall '10 term at Caltech.
- Fall '10