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Preparation of aspirin experiment
Introduction of lab report on aspirin preparation
Introduction of lab report on aspirin preparation
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Recommended: Preparation of aspirin experiment
Aspirin was prepared according to the protocol provided on Blackboard. The three sections to this experiment were 1. Synthesis of Aspirin, 2. Recrystallization of Aspirin, and 3. Characterization of Aspirin. In the first section, the Synthesis of Aspirin, salicylic acid was weight to be 3.029 grams using mass by difference since it was weighed on a 150 milliliter beaker. 9.23 milliliters of the acetic anhydride and 14 drops of 85 percent phosphoric acid were added to this beaker. A Bunsen burner provided by the laboratory was then used to boil the just mixed combination by producing a flame underneath the positioned beaker on top, and then allowed to cool for several minutes after the Bunsen burner flame was terminated. Two quantities of distilled water were then added to this mixture to make it cool even further, which were 41 drops and 30 milliliters. After cooling for some time, this beaker was placed into an ice bath in order to start the crystallization process. A glass rod was used to scratch around the bottom and the sides to catch all of the crystallized Aspirin that was being formed during this whole process. Then, by using a Buchner funnel and filter paper, which was placed on top of the flask connected to a water aspirator with rubber tubing, the excess liquid was removed from the just scraped Aspirin crystals when the Aspirin was placed on the filter paper. Using a medicine dropper, the Aspirin crystals on the filter paper were washed with distilled water just so that any non-pure substances were removed from the crude product. When these crystals were then ultimately dry, they were placed on a watch glass and put into an oven for 30 minutes. Then they were weighed by mass by difference to yield 2.4667 grams of crude s... ... middle of paper ... ...s the change in the temperature of both of these batches, 6°C for the pure, and 13°C for the crude. In this final sub-section of the Characterization of Aspirin, the values of absorbance were recorded. Initially, 0.0566 grams and 0.0590 grams of pure and crude Aspirin respectively were obtained and each individually placed into beakers (400 milliliter) and had 250.0 milliliters of distilled water added to them. From each beaker, a tiny amount of the just dissolved solutions was transferred to a cuvette, one cuvette for each type of aspirin. Each cuvette was placed into the ultraviolent spectroscopy mechanism which was connected to a computer and absorbance spectrum values were obtained at 298 nm (Figure 5) (0.1987 pure aspirin, and 0.9549 crude aspirin). Cumulatively these three methods resulted in the determination of the percent purity for each type of aspirin.
In a separate beaker, acetone (0.587 mL, 8 mmol) and benzaldehyde (1.63 mL, 16 mmol) were charged with a stir bar and stirred on a magnetic stirrer. The beaker mixture was slowly added to the Erlenmeyer flask and stirred at room temperature for 30 minutes. Every 10 minutes, a small amount of the reaction mixture was spotted on a TLC plate, with an eluent mixture of ethyl acetate (2 mL) and hexanes (8 mL), to monitor the decrease in benzaldehyde via a UV light. When the reaction was complete, it was chilled in an ice bath until the product precipitated, which was then vacuum filtrated. The filter cake was washed with ice-cold 95% ethanol (2 x 10 mL) and 4% acetic acid in 95% ethanol (10 mL). The solid was fluffed and vacuum filtrated for about 15 minutes. The 0.688 g (2.9 mmol, 36.8%, 111.3-112.8 °C) product was analyzed via FTIR and 1H NMR spectroscopies, and the melting point was obtained via
For this solution, 5 mL of the solution with 2.5 mL of AMV was placed in the cuvette. The cuvette was placed inside of spectrophotometer and the amount of absorbance was recorded. This procedure that involves a solution with a known concentration was repeated for the concentrations:1.0x10-4 M,5.0x10-5 M,2.0x10-5M, and1.0x10-5M.A unknown solution absorbance was measured by putting 5 mL of unknown solution with 2.5 mL AMV in a cuvette. The cuvette was placed in the spectrophotometer and the amount of absorbance was recorded. The procedure that deals with the unknown solution was repeated 2 more times with the same solution and the same amount of solution and AMV.
The aspirin crystals were packed into 3 small capillary tubes to ensure that they are compressed so as to prevent any air gaps. Subsequently, the aspirin crystals that are in the 3 capillary tubes are placed into the melting apparatus and the temperature range was recorded. Since the range is quite far from the theoretical value of 140°C, aspirin's purity attained was low due to impurities present. One potential reason is because of the swift cooling. When the aspirin is left to cool, the crystal lattices will form too rapidly which will surround other molecules thus making the aspirin impure. Another reason could be because the recrystallized aspirin has not dry completely and there might me left over solvent that will affect the temperature range of the aspirin.
There were some changes in the amount of solvents and products used. For example, 0.5ml of sulfuric acid was used instead of 20ml.
In this lab, Thin Layer Chromatography was used to identify the components of a certain drug. To do this, the compound in question, Motrin was tested against six standards in three different solvents. The three solvent were hexanes, ethyl acetate, and 75% ethyl acetate and 25% hexane; the solution of 75% ethyl acetate and 25% hexane was determined to be the best solvent. This is due to the larger variance in RF values. The six standards that Motrin was tested against were Aspirin, ibuprofen, acetaminophen, naproxen sodium, caffeine and a caffeine and ibuprofen mixture. To determine which standard was present in the chosen drug, the retention factors, or RF, were calculated. A UV light was also used to see the distance each sample traveled in
Following the aforementioned procedure, the neutral compound was to be isolated from the ether solution. Moved to a clean flask, the ether solution was introduced to anhydrous sodium sulfate. After letting the mixture sit for about 10 minutes, the mixture was decanted into a new beaker. The ether in this final mixture was allowed to evaporate, leaving behind the neutral compound. Percent recovery was recorded and the compound was transported to a vial.
A bath was prepared using a 400 mL beaker filled halfway with water. The bath was then sat on a hot plate and lest to boil. 2g of salicylic acid was placed in a 125 mL Erlenmeyer flask with 3 mL of acetic anhydride, and 3 drops of concentrated sulfuric acid. The solutions were mixed and placed in the boiling water bath. The solution was left in the boiling bath for 30 minutes. The 125 mL Erlenmeyer flask was removed and placed on the side to cool to room temperature. Once cooled the solution was placed into a 150 mL Beaker that was filled with 20 mL of ice water. As the beaker was placed in the ice bath, it was simultaneously scraped with a glass rod until crystals formed at the bottom of the beaker. The crystal solution was poured into a Buchner
To test the synthesized aspirin, three test tubes were taken, and 1-mL of 95% ethanol and 1 drop of 1% iron (III) chloride solution were added to all the three test tubes. Salicylic acid was added to test tube A, a few crystals of the synthesized aspirin was added to test tube B, and test tube C was used as a control test tube. Each test tube was stirred using a glass stirring rod and the results were recorded. The solutions were then poured into the “Discarded Test Solution” containers.
In the late 1800’s it was discovered that papa-amino-phenol, could reduce fever, but the drug was too toxic to use. A less toxic extract called phenacetin was later found to be just as effective but also had pain-relieving properties. In 1949, it was learned that phenacetin was metabolized into an active but also less toxic drug, acetaminophen. Since then, acetaminophen has been sold under many over the counter brand names, most popular being Tylenol.
After creating the compound acetyl salicylic acid, it will be thoroughly analyzed through a series of steps that test its melting point, purity, and solubility as compared to commercial aspirin. By solving for the melting point range of the synthesized aspirin, one can determine its purity. Then by adding 1% ferric chloride, the color of both the synthesized and commercial aspirin represents its purity. In theory, the synthesized aspirin should be relatively the same color as the commercial drug. Finally, both types of aspirin are placed into different solutions to determine their solubility properties. For all three of these analyses, the synthesized aspirin should test similar to the commercial aspirin in hopes it was created
Part 4 of this lab showed a way to observe impurities by comparing the melting point of crude and pure samples. Since impurities are to be shown in the crude sample it would have a lower melting point and larger range. The known melting point of aspirin is to be 135 oC. The crude sample had a melting point range from 69oC to 81 oC. While the Pure sample melting point range was from 116oC to 125oC. Since the Pure sample was still below 135 oC, this shows that there are still some impurities
This test was carried out by choosing three tablets from each formulation after weighing them. The temperature of the dissolution apparatus was adjusted at 37°C and the speed of paddles was constant at 50rpm.After that, each vessel of the dissolution apparatus was full with 1 liter of phosphate buffer. Subsequently, each tablet was placed into its individual vessel. The test was performed over 8 hours with extracting 10mL of each sample and replaced with the same amount of the phosphate buffer which was at the same temperature over the 8 hours as the following: half an hour, one hour, two hours, three hours, four hours, five hours, six hours, seven hours and eight hours. The all withdrawn samples were analyzed by using the UV spectroscopy
The purpose of the experiment was to acetylate aniline with the use of acetic anhydride and purify the crude acetanilide by recrystallization; in addition, determine the percent yield for acetanilide.
As such, 3 Mmol of cyclohexanone and p-fluorbenzaldehyde were each added to a 100 mL round bottom flask with 30 mL of 10% sodium hydroxide. The reaction was stirred with a magnetic stir rod and allowed to react at room temperature for 1 hour. To determine reaction progress, TLC (figure 3) was performed at 30 minutes, 45 minutes and 60 minutes post reaction start time. After the 60 minute TLC was performed, the reaction was determined to be complete. The product was then separated through a liquid-liquid extraction process. To separate the product, 10 mL of hexanes were added to the reaction and the solution was transferred to a separatory funnel. Then, 10 mL of distilled water were added to the funnel which was then shook vigorously and allowed to settle. The water layer was then drained from the vial and this process was repeated in triplicate. The resulting hexane layer was determined to contain the product of the reaction and was transferred to a 50 mL
The physical studies were designed to ensure the stability of final formulation. The physical mixture of drug and lipids in the ratio of 1:1 was placed in glass vials, sealed and stored in 40ºc and 75% RH. The sample were withdrawn at pre determine time intervals of 15 and 21 day and examined for physical and chemical integrity of drug and Excipient. Parameter such as colour, odour or gas formation and aggregation were noted.