If acetylsalicylic acid does not begin to crystallize out, scratch the walls of the flask with a glass rod. Unless otherwise noted, LibreTexts content is licensed by CC BY-NC-SA 3.0. Submit the crystalline sample in a small vial with proper labeling to your instructor. Ferric Chloride Test For Aspirin. This shows that both the products were relatively pure. Add 10 drops of aqueous 1% ferric chloride solution to a test tube containing a few crystals of the compound to be tested dissolved in 5 mL water and note the color. To confirm that the final product of the synthesis was aspirin, an IR spectrum of the product was taken. Polyesters are often made from dicarboxylic acids and diols. For the reaction to go reasonably fast and to completion, sodium hydroxide is added in excess to ensure the maximum amount of methyl salicylate reacts. Introduction: The purpose of this lab was to learn how to use salicylic acid to make aspirin. http://en.wikipedia.org/wiki/Nucleophilic_acyl_substitution. Another source of product loss was during the filtration of the product. When the product is completely dry, weigh its weight, determine its melting point (lit mp 135 °C) and calculate the percentage yield of this recrystallized product. The ferric chloride test was used to compare the salicylic acid, crude aspirin, and purified aspirin. Clamp a side-arm flask to the ring stand, and connect a piece of rubber tubing to the side-arm. … The sample is dissolved in water, or a mixture of water and ethanol, and a few drops of dilute ferric chloride (FeCl3) solution is added. 1) Ferric Chloride Test The addition of ferric chloride to salicylic acid produces a specific color caused by the reaction of salicylic acid with aqueous ferric (Fe(H the -OH group on the salicylic acid together can form a complex with Fe(H an intense violet color. During this semester, you will have an opportunity to isolate some pharmacologically active natural products and to synthesize other active compounds from suitable starting materials. The final test tube should be a blank and have nothing but the alcohol and ferric chloride … Register now! Normally, you measure reactants to at least two significant figures. Methyl Salicylate is a naturally occurring chemical that is obtained from winter green oil that can be used to synthesize Salicylic Acid. This complex has an intense colour, which may vary from blue, green or even red depending upon the nature of the phenol. Enols, hydroxamic acids, oximes, and sulfinic acids give positive results as well. 1.600g of aspirin was obtained after the second synthesis. In the case of quick qualitative detection of acetyl salicylic acid and salicylic acid a simple visual test will suffice. The aspirin was obtained with 58.75%. To help push the reaction toward the products, one could distill off the acetic acid. University of Missouri–St. One possibility for loss of product could be during the acidification step. Phenols form a complex with ferric ions. The salicylic acid was obtained with 76.5% yield so there are sources of product loss. This was a white powder and had a melting point range of 134-135 degrees Celsius.

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