Synthesis and Characterization of Aspirin Product Identity and Purity After synthesizing a

An Erlenmeyer flask was used to accommodate the largest volume of recrystallization solvent calculated and was cooled in an ice bath to increase the yield of crystals. The solid was collected by vacuum filtration and washed with a small amount of ice water. The product is then dried to a constant mass by use of an oven and weighed. A small amount of the unknown was compared to two samples of acetanilide and phenacetin for a melting point range to determine the identity. The temperature of the unknown was recorded when the first trace of liquid can be seen and when the unknown was completely liquid.

Aspirin, Caffeine and Salicylamide were extracted from an over-the-counter pain reliever (BC Powder). These components were separated by manipulating their solubilities by adjusting the acidity and basicity of the solution. By doing this, the three components were forced into conjugate acid (or base) forms, causing selective solubility in either an aqueous or organic solvent. These layers were then separated by use of a separation funnel. Once separated, the components extracted were characterized by measuring the melting point and performing a TLC analysis. Also, the recovered aspirin from the first part of the experiment was recrystallized and compared to that of the

2. Used a test tube clamp to held the test tube and gently heated the tube in a laboratory burner flame for about 30 seconds.

The vial was removed from the heat and cooled to room temperature. The spin vane was rinsed with 2-3 drops of warm water over the conical vial. The vial was cooled to room temperature then placed in an ice bath for 15 minutes. The liquid was decanted from the mixture and the resulting crystals were dried on filter paper. The crystals were then placed on a watch glass for further drying. The crystals were weighed and a small sample was placed into a capillary tube for melting point determination.

The aspirin was synthesized when it was placed in a cold bath. Purification was necessary to remove any unreacted salicylic acid and acetic anhydride as well as the acetic product and phosphoric acid. Acetic acid and phosphoric acid are water soluble so they were removed by

The goal of this experiment was to synthesize aspirin. In this experiment aspirin, also known as acetylsalicylic acid, was synthesized from salicylic acid and acetic anhydride. In the reaction the hydroxyl group on the benzene ring in salicylic acid reacted with acetic anhydride to form an ester functional group. This method of forming acetylsalicylic acid is an esterification reaction. Since this esterification reaction is not spontaneous, sulfuric acid was used as a catalyst to initiate the reaction. After the reaction was complete some unreacted acetic anhydride and salicylic acid was still be present in the solution as well as some sulfuric acid, aspirin, and acetic acid. Crystallization, which uses the principle of

24) Separate the formed crystals (benzoin) and allow them to dry, then take the MP.

Both Aspirin and the Unknown are soluble in dichloromethane, due to their non-polar characteristics. To separate the two components, sodium bicarbonate was added (see figure 3). Sodium bicarbonate reacted with aspirin and converted it to a salt, also forming water and carbon dioxide. It was observed that the solution "fizzed" when this reaction took place, showing the release of carbon dioxide. The newly formed salt then traveled to an aqueous layer where it was soluble, while the unknown remained in the dichloromethane layer. The two layers were then separated. To collect an aspirin solid, the combination of the addition of HCl and the process of vacuum filtration helped to break down the salt and form a solid. Then the solid was placed in the Fisher Scientific Biotemp Oven to dry it to a constant mass of 0.091 g, 32.97% of the total composition. The

The purpose of this lab was to synthesize aspirin, determine the theoretical yield, compare the percent yield to the theoretical yield and test the purity of aspirin by adding Iron (III) chloride to the product.

11. During the 10 minutes, get the LB agar and LB+AMP agar plates ready. Mark your plates with the transformation tube mixture to use (+ or -), the lab group names, and the date on the top of the dishes.

4.Measure 35mL of warm water and add them into each of the 4 test tubes at about roughly the same time. It is essential that the water is warm. Do not seal the test tube.

To tube 2 and tube 3 a boiling chip is added. The two tubes are boiled to remove any residual ether. Next, the tubes are cooled to room temperature and placed into an ice bath to allow for crystallization. The solution is then removed from the solid in each tube and discarded. To tube 2 and 3 ~0.5 ml of H2O is added for recrystallization, the tubes

In this experiment, acetylsalicylic acid or aspirin was synthesized by the esterification reaction between salicylic acid and acetic anhydride. This esterification reaction consisted of acetic anhydride with a carboxylic acid functional group and salicylic acid with an alcohol functional group making acetylsalicylic acid, which contains an ester functional group. Sulfuric acid was used as a catalyst to make the products of acetic anhydride and acetic acid. The experimental technique of crystallization was used to purify acetylsalicylic acid from other substances, because when the esterification reaction was complete some unreacted salicylic acid and acetic anhydride was present along with acetylsalicylic acid, acetic acid, and the catalyst: sulfuric acid.

This report presents the synthesis of Aspirin (acetylsalicylic acid), as the product of the reaction of salicylic acid with ethanoic anhydride under acidic conditions. Aspirin was purified through recrystallisation by vacuum filtration, followed by desiccation of the Aspirin crystal over silica gel. The percentage yield was calculated as 44.89% and a sample of Aspirin was analysed using infra-red spectroscopy and compared to the spectrum of pure Aspirin, this served as an introduction to the identification of functional groups in organic compounds. The melting point was calculated using an IA9000M apparatus and recorded to be 35.2°C, which was slightly below the melting point of pure Aspirin; known to be between 138-140°C. Both IR spectroscopy and melting point measurement were used verify the purity of synthetic Aspirin made, which proved to be fairly pure under these laboratory conditions.

Once the range is obtained, remove the thermometer and beaker. Pour out the hot water and allow both the thermometer and the beaker to cool. Once cool, repeat the previous steps with the second compound, tetradecanol. At the conclusion of the second experiment, repeat the steps for a third and final time using an equal mixture of both compounds. Be sure to record the melting point range for all three experiments.