Question

PROCEDURE 1. Place a reaction tube into a 5-mL Erienmeyer and tare. Add between 0.275- 0.300g of salicylic acid. Record on the data sheet. 2. Transfer the reaction tube and 5-ml Erienmeyer to the hood. Add a boiling chip, 2 drops of 85% phosphoric acid, and about 0.70 mL of acetic anhydride to the reaction tube. Mix well. 3. Place a 50-ml beaker containing about 20-mls of water on a hot plate or in the sand bath. Allow the water to become hot (390*C). Then, place the reaction tube in the hot water bath for at least five minutes. 4. In 5-drop increments, add about 1-mL of water. This serves to decompose any excess acetic anhydride, producing acetic acid. Since the acetic acid vapors can be quite strong, it is important to do this in the hood. Since this hydrolysis is exothermic, the reaction is over when the reactants begin to cool down. 5. Allow the reactants to cool slowly to room temperature. At this stage, crystals of acetylsalicylic acid should begin to form. If no crystal formation is observed, use the standard techniques start crystallization. 6. Cool thoroughly in an ice bath for at least ten minutes. 7. Suction filter using the Hirsch funnel. Use a very small quantity of ice-water to wash and help transfer the crystals. 8. Press dry. Weigh and obtain the melting point. Record on the data sheet. 9. Obtain the IR of a chloroform solution of the product if time permit?.