Introduction The purpose of this experiment was to purify acetanilide that was contaminated with relatively small amounts of impurities using recrystallization. The success of recrystallization was dependent on a suitable solvent being chosen and proper recrystallization technique being carried out. The solvent chosen had to have a different polarity than that of the molecule of interest. The technique used was dependent on the solubility of the solvent at higher temperature and the solubility of the impurities at all temperatures. To analyze the acetanilide product of the reaction, 1H NMR and IR were used. Results, Discussions, and Conclusions In this experiment, acetanilide was synthesized via nucleophilic acyl substitution from both acetic anhydride and aniline. During this reaction, aniline acts as the nucleophile and acyl (CH3CO-) group from acetic anhydride acts as the electrophile. The hydrogen atom of –NH2 group is replaced by the acyl group. The crude product contained acetanilide, and acetic acid, which was the impurity. Recrystallization, which was used to purify the contaminated acetanilide, required a suitable hot solvent which dissolved all the crude product, but upon being cooled, since …show more content…
The melting point range for the crude product was 113-115.3℃. the melting point range for the purified product was also 113-116℃. This melting point range was almost perfect to that of the theoretical melting point which is 113-115℃ proving that the product was in fact created. When looking at the percent yield of the crude acetanilide, there was an 81% yield which was a very good yield because the average percent yield is between 80-90%. The percent recovery of the acetanilide was 88% which is also very good because much of the product was recovered meaning that the product was in fact
1mL of Acetic acid was then added to Unknown D and the solution was stirred. Next, 15mL of sodium
The unknown compound was first reacted with an acid. To begin, 0.50 grams of KCl was mixed with 5 mL of water. Then, 1 mL of 6 M H2SO4 was added to the solution. Secondly, the unknown compound was reacted with a base. Exactly 0.50 grams of KCl was mixed with 5 mL of water, and 1 mL of 1 M NaOH was added to the solution next.
In April 15, 2010 the Reed Richards Science Center in Akron burned to the ground. The Center had been conducting controversial cosmic ray experiments on rats and rabbits, and a number of animal rights groups had opposed the research. Preliminary investigations by the FBI’s Special Crimes Unit determined that there was a high level of Acetone found in the debris after the fire. Acetone is a highly flammable accelerant that can be used to help fires spread quickly through buildings. It is very rare and its distribution is tightly controlled by federal regulations.
The purpose of this experiment was to learn about the electrophilic aromatic substitution reactions that take place on benzene, and how the presence of substituents in the ring affect the orientation of the incoming electrophile. Using acetanilide, as the starting material, glacial acetic acid, sulfuric acid, and nitric acid were mixed and stirred to produce p-nitroacetanilide. In a 125 mL Erlenmeyer flask, 3.305 g of acetanilide were allowed to mix with 5.0 mL of glacial acetic acid. This mixture was warmed in a hot plate with constantly stirring at a lukewarm temperature so as to avoid excess heating. If this happens, the mixture boils and it would be necessary to start the experiment all over again.
Benzyne Formation and the Diels-Alder Reaction Preparation of 1,2,3,4 Tetraphenylnaphthalene Aubree Edwards Purpose: 1,2,3,4-tetraphenylnaphthalene is prepared by first producing benzyne via the unstable diazonium salt. Then tetraphenylcyclopentadienone and benzyne undergo a diels-alder reaction to create 1,2,3,4-tetraphenylnaphthalene. Reactions: Procedure: The reaction mixture was created. Tetraphenylcyclopentadienone (0.1197g, 0.3113 mmol) a black solid powder, anthranilic acid ( 0.0482g, 0.3516 mmol) a yellowish sand, and 1,2-dimethoxyethane (1.2 ml) was added to a 5-ml conical vial.
Lab Report 5: Acetylsalicylic Acid (Aspirin) Synthesis Name: Divya Mehta Student #: 139006548 Date Conducted: November 19th 2014 Date Submitted: November 26th 2014 Partner’s Name: Kirsten Matthews Lab Section: Wednesday 2:30 L9 IAs Name: Brittany Doerr Procedure: For the procedure, see lab manual (CH110 Lab Manual, Fall 2014) pages 96-98. Wilfrid Laurier University Chemistry Department. Fall 2014. Acetylsalicylic Acid (Aspirin) Synthesis.
9. The melting point range was lower than the given range of the anti-addition product by 2 degrees Celsius. This could have been due to impurities in the product. A likely cause could have been water that still remained in the product after recrystallization (the product shifted upward during melting point analysis due to evaporation). Since water has a low melting point, it could have lowered the melting point range of the product.
The purpose of this experiment is to perform a two step reductive amination using o-vanillin with p-toluidine to synthesize an imine derivative. In this experiment, 0.386 g of o-vanillin and 0.276 g of p-toluidine were mixed into an Erlenmeyer flask. The o-vanillin turned from a green powder to orange layer as it mixed with p-toludine, which was originally a white solid. Ethanol was added as a solvent for this reaction. Sodium borohydride was added in slow portion as the reducing agent, dissolving the precipitate into a yellowish lime solution.
We were able to eliminate certain ingredients like chlorpheniramine because this ingredient was the only neutral and the properties were not similar to the unknowns. The other team identified that the unknowns included all the ingredients except for the acetylsalicylic acid. They came up with their conclusions based off during the starch test both unknowns contained starch. They had different results than our team during the acetone solubility test. Team 2 found that both unknowns were acetone soluble, but our team found only unknown B was acetone soluble.
The purpose of this experiment was to learn about metal hydride reduction reactions. Therefore, the sodium borohydride reduction of the ketone, 9-fluorenone was performed to yield the secondary alcohol, 9-fluorenol. Reduction of an organic molecule usually corresponds to decreasing its oxygen content or increasing its hydrogen content. In order to achieve such a chemical change, sodium borohydride (NaBH4) is used as a reducing agent. There are other metal hydrides used in the reduction of carbonyl groups such as lithium aluminum hydride (LiAlH4).
The main objective of this experiment was the formation of phenacetin from the synthesis of acetaminophen. This was done through a chemical reaction known as the Williamson ether synthesis using techniques of refluxing, vacuum filtration and recrystallization incorporating a mixed solvent system. A further objective of this experiment was to study the formation of the product (phenacetin). Such validation was completed by using techniques for determining the melting point, calculating percent yield, and IR (infrared spectroscopy) of the resultant product.
The substitution reaction was successful but not fully effective. 19. If the data was inconclusive, then comparing various compounds and the unknown based on physical characteristics would be the first step, titrations would also be a good method. 20. To get a better yield, redoing the experiment would require careful attention in the recrystallization steps: amount of solvent used, how hot solvent is, if the mixture cools to room temperature before placing it in an ice
This supports the isolated product is majority made of the desired product and is largely pure. Mass spectrometry of the crude product shows the molecular ion peak is 162.1, which is the largest fragment in the mass spectrum (Figure 4) and corresponds to the molecular weight of methyl trans-cinnamate (Table 1). The base peak is 131, inferring the fragment lost is 31 m/z in size. This 31 m/z matches the OCH3 fragment of the ester, and would not result from a trans-cinnamic acid. This is evidence the product was successfully
The percent yield was 22.33%. In most cases, that means that a lot of possible product was lost. However, in this case, that was not true. When Benzaldehyde reacted with the Wittig reagent, it produced two products: E-Stilbene and Z-Stilbene. The Z product was a liquid, while the E product was a solid.
Purpose/Introduction The process of recrystallization is an important method of purifying a solid organic substance using a hot solution as a solvent. This method will allow the separation of impurities. We will analyze Benzoic Acid as it is dissolved and recrystallized in water and in a solvent of Methanol and water. Reaction/Summary