ORGANIClab2 - E xperiment N o.: 2 Name: Paul Gonzales...

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Experiment No.: Experiment Name: Date: 2 Separation of the Component of Penacetin 06/18/10 Name: Course: Paul Gonzales CH 2123 1
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Purpose: to separate the components of a simulated pharmaceutical preparation, Panacetin, making use of their solubilities and acid-base properties. Physical Data: MW Mp Bp Density Solubilit y Hazards Sucrose Ins. in H20 Asprin Ins In H20 Dichloromet h. Deadly API – Active Pharmaceutical Ingredient Sucrose is insoluble in dichloromethane Asrpin, acetanilide, and phenacetin are soluble in dichloromethane Asprin reacts with bases (sodium bicarbonate) to form a salt – sodium acetylsalicylate, which is insoluble in dichloromethane and soluble in water Acetanilide and phenacetin are not converted to salts by sodium bicarbonate Panacetin: 50% acetanilide or phenacetin, 40% Aspirin, 10% sucrose Calculations: N/A Procedure: 1. Weight 3.00 g of Panacetin and transfer to clean, dry 125-mL Erlenmeyer flask. Add 50 mL dichloromethane to flask. Stir. Preweigh filter. 2. Filter the mixture using filter paper, set the filter paper aside being careful not to lose any of the sucrose. Reweigh when completely dry. 3. Record the mass of the sucrose in lab notebook. 2
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4. Transfer filtrate to separatory funnel and extract it with two separate 30-mL portions of 5% sodium bicarbonate. For each extraction, use a stirring rod to stir the liquid layers until any fizzing subsides before you put a stopper and shake the separatory funnel. 5. Transfer each layer to a different container and label. Return the dichloromethane layer for the separatory funnel before the second extraction. Combine the two aqueous extracts in the same container and save the dichloromethane layer for the next step. 6. Add 7.0 mL of 6 M hydrochloric acid slowly to the combined aqueous extracts while stirring with a glass rod. Test the pH of the solution, and add more acid, if necessary to bring the pH down to 2 or lower. Cool the mixture in an ice/water bath for at least 10 minutes, collect the aspirin by vacuum filtration, and wash it on the filter with cold water. 7. Let the aspirin dry on the filter for a few minutes with the aspirator running, then dry it to constant mass. Weigh the aspirin and record its mass. 8. Use a filter flask attached to a trap and aspirator to evaporate
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This note was uploaded on 09/07/2010 for the course CHEM CH 2123 taught by Professor Heemoonpark during the Summer '10 term at Austin Community College.

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ORGANIClab2 - E xperiment N o.: 2 Name: Paul Gonzales...

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