Chemistry : Melting Points Were Obtained With An Electro Thermal Digital Melting Point Apparatus ( Model 9100 )

Melting Point Data Table Compound Aspirin Caffeine Salicylamide Actual MP (ºC) 93 - 98 260 - 262 96 - 102 Expected MP (ºC) 135 236 140 Percent Error (%) ~30% ~12% ~30%

The mixture was transferred to an ice bath to crystallize the product, after which the product was collected by vacuum filtration on a Hirsch funnel, washing the flask with small aliquots of cold xylene and pouring the solution over the crystals, allowing the vacuum to thoroughly dry the product. Additional drying was achieved by transferring the product to filter paper and pressing the crystals to remove any excess moisture. The product was then weighed and a melting point determined. A comparative TLC was run in Hexanes:Ethyl Acetate solvent against maleic anhydride to verify the purity of the

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

4- chlorobenzoic acid which was the aqueous layer has a theoretical melting point of 240-243°C, the organic layer, 4-chlorobenzyl alcohol has a theoretical melting point of 68-71°C. During our experiment we were unable to collect any data for the organic

After 10 minutes the reaction liquid was separated from the solid using a vacuum filtration system and toluene. The product was stored and dried until week 2 of the experiment. The product was weighed to be 0.31 g. Percent yield was calculated to be 38.75%. IR spectra data was conducted for the two starting materials and of the product. Melting point determination was performed on the product and proton NMR spectrum was given. The IR spectrum revealed peaks at 1720 cm-1, which indicated the presence of a lactone group, and 1730 cm-1, representing a functional group of a carboxylic acid (C=O), and 3300cm-1, indicating the presence of an alcohol group (O-H). All three peaks correspond with the desired product. A second TLC using the same mobile and stationary phase as the first was performed and revealed Rf Values of 0.17 and 0.43for the product. The first value was unique to the product indicating that the Diels-Alder reaction was successful. The other Rf value of 0.43 matched that of maleic anhydride indicating some

Using SN1 reaction mechanism with hydrochloric acid, t-Pentyl alcohol was converted to t-Pentyl chloride in an acid catalyzed reaction. The reaction took place in a separatory funnel designed to separate immiscible liquids. The crude product was extracted by transferring a solute from one solvent to another. The process of washing the solutions by phase transfer was used in order to remove impurities from the main solvent layer. Finally, the crude product was dried with anhydrous Calcium chloride and purified once more by simple distillation technique.

Seven test tubes were labeled numerically with 2 mL of VO3- and H2SO42- added to each tube. A small pea size portion of solid Na2SO3 was added to the first test tube. Then, 20 drops of distilled water were added to the second test tube. In the third test tube, 20 drops of (.2 M) NaBr were added. Then, to drops of (.2 M) NaNO2 were added into the fourth test tube. A small portion of Fe(NH4)2(SO4)2 * 6H2O was added into the fifth test tube. The sixth test tube had 20 drops of (.2 M) H2Cr2O4 added, where the seventh test tube was the control tube with no additional chemicals added. All the test tubes were left to react for 3 minutes and then heated in a heated bath for approximately 20 minutes.

Discussion: As seen in the melting point determination, the average melting point range of the product was 172.2-185.3ºC. The melting points of the possible products are listed as 101ºC for o-methoxybenzoic acid, 110ºC for m- methoxybenzoic acid, and 185ºC for p- methoxybenzoic acid. As the melting point of the sample

Aim: To classify unknown substances according to their structure type and to observe how the structure of materials affects their uses.

The objective of this lab is to synthesize acetaminophen from p-aminophenol. The techniques used to do so, consist of: reflux with heat to allow reaction to occur at a reasonable time period, extraction and filtration to isolate the desired product, and characterization of the product by analyzing IR spectras and melting points. Acetaminophen considered synthesized, primarily due to the IR spectrum exhibiting all the bond vibrations is the amide group. The percent yield of 124.6% imply that there was a mechanical error that occurred, thus, also tampering with the progression of the chemical reaction. The wide melting point range of 165 C-169 C denote the impurity of the acetaminophen product.

As the acid was being added, the mixture was being stirred over a stir plate. Once completed, the reaction mixture was poured from the round bottom flask into a 500 mL separatory funnel and its top (organic) layer was extracted into another beaker. The bottom (aqueous) layer was placed back into the funnel and extracted twice with 50.0 mL of ethyl ether each. The newly extracted layers were combined and dried over magnesium sulfate (MgSO4). The dried solution was the decanted into a beaker to remove the MgSO4 salts and the product solution was collected via Buchner vacuum filtration. The resulting product was transferred into an Erlenmeyer flask with an inverted beaker on top and stored in a drawer.

outline the steps and conditions necessary for the industrial production of H2SO4 from its raw materials

2-Applied Physical and Analytical Chemistry Laboratory, Department of Inorganic Chemistry, P.O Box 812 Yaoundé, University of Yaoundé I - Cameroon