Chemistry 30A3 Fall 2011 Labs Dr. Troendle 61

Chemistry 30A3 Fall 2011 Labs Dr. Troendle 61 - mL round...

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Chemical Biology 3OA3, September 2009 Page 61 OH O H O- Na+ O- Na+ O- Na+ O- Na+ O O O O- Na+ O O OEt OEt O- Na+ O O OEt O- Na+ O O OEt O O O OEt O O O O O O H O O- Na+ O O O O- Na+ 1. -OEt 2. 3. 4. -OEt H 3 O + during work-up This experiment will be done on milligram scale, using microscale equipment and techniques. Before coming to the lab, be sure to read the sections on microscale distillations, extractions, and recrystallizations in "Microscale Laboratory Techniques" after this lab. Microscale Preparation of 4-Hydroxycoumarin Note: It is very important that all equipment used in this reaction be thoroughly dried in an oven at 110 o C for 30 minutes just prior to use. Upon removal from the drying oven, it should be allowed to cool to room temperature in a desiccator. Weigh and place 85 mg (2.13 mmol) of sodium hydride (60% dispersion in mineral oil) in a 10-
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Unformatted text preview: mL round bottom vial containing a magnetic stirring bar. Now add 3.0 mL of dry toluene. To the flask attach a Hickman still fitted (at the top) with a condenser protected (again, at the top) by a calcium chloride drying tube. CAUTION : Sodium hydride (NaH) is a flammable solid which reacts violently with water to produce hydrogen gas. Dispense in the hood . Toluene is distilled and stored over molecular sieves. Dispense this solvent in the hood as well. IMPORTANT NOTE: Use the right stuff: sodium hydride is in the SMALL BOTTLE inside the larger bottle. The large bottle is a dessicant to keep the NaH dry. This reaction...
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This note was uploaded on 01/08/2012 for the course CHM 30A3 taught by Professor Ricktroendle during the Fall '11 term at UNF.

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