Synthesis And Characterization Of Aspirin

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

Separation and Purification of the Components of an Analgesic Tablet. Cora Bruno, Lab Section E. Aspirin, Caffeine and Acetaminophen were separated from four analgesic tablets of Excedrin using extraction techniques. 5% wt/vol NaHCO3, 4M HCL, ethyl acetate and deionized water were used to separate the three active components. MgSO4 was used to dry each extraction. Aspirin was isolated using a hot water bath and weighed to determine the percent theoretical recovery and the actual percent recovery of aspirin. After separation, Aspirin (ASA), Caffeine (CAF), and Acetaminophen (ACE) were purified and identified using Thin Layer Chromatography (TLC). Standards and purified ASA, CAF, and ACE were spotted on the silica gel (stationary phase) of the

14 mL of 9 M H2SO4 was added to the separatory funnel and the mixture was shaken. The layers were given a small amount of time to separate. The remaining n-butyl alcohol was extracted by the H2SO4 solution therefore, there was only one organic top layer. The lower aqueous layer was drained and discarded. 14 mL of H2O was added to the separatory funnel. A stopper was placed on the separatory funnel and it was shaken while being vented occasionally. The layers separated and the lower layer which contained the n-butyl bromide was drained into a smaller beaker. The aqueous layer was then discarded after ensuring that the correct layer had been saved by completing the "water drop test" (adding a drop of water to the drained liquid and if the water dissolves, it confirms that it is an aqueous layer). The alkyl halide was then returned to the separatory funnel. 14 mL of saturated aqeous sodium bicarbonate was added a little at a time while the separatory funnel was being swirled. A stopper was placed on the funnel and it was shaken for 1 minute while being vented frequently to relieve any pressure that was being produced. The lower alkyl halide layer was drained into a dry Erlenmeyer flask and 1.0 g of anhydrous calcium chloride was added to dry the solution. A stopper was placed on the Erlenmeyer flask and the contents were swirled until the liquid was clear. For the distillation

The mixture was heated at 120°C using an aluminum block and was stirred gently. After all of the solid dissolved, it was heated for 20 additional minutes to ensure the reaction was complete.

3.0g of salicylic acid was weighed then 3.0mL of acetic anhydride and 6 drops of 85% H3PO4 were added to it. The mixture was warmed over a water bath for 5 minutes while stirring. After warming, 20 drops of distilled water was slowly added. 15mL of water was added then the solution was heated until it became clear. It was allowed to cool and was placed in an ice bath until the solution becomes cloudy. Using pre-weighed filter paper, the mixture was filtered and was allowed to dry in the filter paper.

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

Aspirin is one of the most consumed painkillers created up to this date due to its reliability and low expense. It is often used to relieve minor aches and pains, reduce fever and as an anti-inflammatory medication. Due to its wide range of uses, the demand for this pharmaceutical is very high. As a result, manufacturers who produce this drug must be efficient in order to reduce the time taken to produce this drug and produce the in very high quantities.

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.

The wet, crude product was placed into the 50 mL Erlenmeyer flask. Small amounts of CaCl2 were added to dry the solution. The flask was sealed and the mixture was swirled and left to settle. Once

The next day an orange goopy textured product resulted. The extracts were then dried and combined with anhydrous sodium sulfate, then evaporated with dry air under the hood in a warm water bath. The liquid was cooled and had an initial weighing of 0.5887g. It was reweighed several minutes later with a final

40 g of ice and approximately 30 ml of sulfuric acid is cautiously added to a 100 mL beaker respectively. Weigh 7.6 g of ammonium chloride and 14.0 g of ammonium bromide and place it in another beaker, crushing the lumps until a powdery mixture remains. The powdery mixture is then transferred to a 125 mL Erlenmeyer flask. Add the ammonium salts into the sulfuric acid mixture. Heat is applied to dissolve the salt. Once the

After the mixture finished refluxing, the flask was then cooled on ice. A sulfuric acid solution was then prepared by pouring 4.5 mL of concentrated H2SO4 over 50 grams of ice and then diluted to 75 mL by adding enough tap water to reach 75 mL. The sulfuric acid solution was then cooled on ice.

Cold NaOH solution (0.2 mol NaOH in 7 mL H2O) was slowly added and the mixture was stirred for 5 h. The resulting slurry was dried at 100 °C for 24 h, and calcined at 700 °C for 60 min. After cooling to room temperature, the

A historical Development that relates to Aspirin is the father of our modern Medicine Hippocrates, who was a Greek Physician, left records of how they treated headaches, fevers and pains, and to ease child- bearing pains with a powder made of the leaves and bark form a Willow Tree. Also the Ancient Egyptians left a medical text called “Ebers Papyrus” which is also lists willow among a list a plant and animal remedies for pain relief, fever reduction, and as an anti-inflammatory. Also the Roman Celsus recommended Willow extract for treating the symptoms of Inflammations, swollen, red, feverish area, and pain. (Wikipedia “history”) This is relatable as the bark and leaves of the Willow tree are a natural resource of the Salicylic acid, which is found in Aspirin, which made the patients feel better while healing them, similar to the modern Aspirin. Further along in Human history we know that Edward Stone discovered and isolated the key chemical in the Willow bark/leaves called Salicylic Acid. The problem with the Salicylic acid was that it was extremely tough on stomachs and could cause nausea and vomiting, hence the next step in developing Aspirin was to find an effective buffer that would make the Salicylic acid easier for the stomach to handle, a French chemist named Charles Frederic Gerhardt was one of the first to attempt at creating a suitable buffer for Salicylic acid was to combine it with Sodium and Acetyl Chloride,

Headache medicine is a non steroidal mitigating drug,Pain relieving diminishes torment, utilized for the help of migraines and a throbbing painfulness. Calming in higher measurements utilized for the treatment of provocative conditions, for example, joint inflammation.