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What is the proper procedure for synthesizing aspirin from salicylic acid and acetic anhydride, and how can the purity of the final product be assessed and improved?

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Synthesizing aspirin  acetylsalicylic acid  from salicylic acid and acetic anhydride involves a process called acetylation. Here is a general outline of the procedure:1. Preparation:   - Gather necessary materials: salicylic acid, acetic anhydride, concentrated sulfuric acid  catalyst , ice bath, vacuum filtration setup, and appropriate glassware.   - Ensure all glassware is clean and dry.2. Synthesis:   - In a dry Erlenmeyer flask, add a measured amount of salicylic acid  e.g., 5 grams .   - Add a slight excess of acetic anhydride to the flask  e.g., 7 mL .   - Add a few drops of concentrated sulfuric acid as a catalyst to speed up the reaction.   - Gently swirl the flask to mix the contents and let the reaction proceed for about 15-20 minutes at room temperature.   - While the reaction is taking place, prepare an ice bath in a beaker or container.3. Quenching the reaction:   - After the reaction time has passed, slowly add cold water to the flask to quench the reaction and precipitate the aspirin. The addition of water will also hydrolyze any excess acetic anhydride.   - Place the flask in the ice bath to further cool the mixture and promote crystallization of the aspirin.4. Filtration and washing:   - Set up a vacuum filtration system with a Büchner funnel and filter paper.   - Filter the aspirin crystals from the reaction mixture, using the vacuum to help draw the liquid through the filter.   - Wash the crystals with a small amount of cold water to remove any remaining impurities, such as unreacted salicylic acid or acetic acid.5. Drying and weighing:   - Transfer the aspirin crystals to a clean, dry watch glass or weighing paper.   - Allow the crystals to air dry or use a gentle heat source  e.g., a drying oven  to remove any remaining moisture.   - Weigh the dried aspirin crystals to determine the yield of the synthesis.To assess the purity of the synthesized aspirin, you can use the following methods:1. Melting point determination:   - Determine the melting point of the synthesized aspirin using a melting point apparatus.   - Compare the observed melting point to the known melting point of pure aspirin  135-136C . A lower or broader melting point range may indicate impurities.2. Thin-layer chromatography  TLC :   - Perform a TLC analysis of the synthesized aspirin, comparing it to a standard sample of pure aspirin and salicylic acid.   - The presence of impurities or unreacted starting materials will be indicated by additional spots on the TLC plate.To improve the purity of the final product, you can recrystallize the aspirin:1. Dissolve the synthesized aspirin in a minimal amount of hot ethanol or another suitable solvent.2. Slowly add hot water to the solution until it becomes cloudy.3. Allow the solution to cool slowly to room temperature, and then cool further in an ice bath to promote crystal formation.4. Filter the recrystallized aspirin using vacuum filtration, wash with cold water, and dry as before.5. Reassess the purity using melting point determination and/or TLC analysis.
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