The Use Of Glycerol Residue

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

The goal of this was to successfully accomplish the synthesis of para-Chlorophenoxyacetic acid. In this experiment, para-Chlorophenoxyacetic acid was synthesized from 4-chlorophenolate and chloroacetic acid using an SN2 reaction. The product obtained was determined to be the para isomer of Chlorophenoxyacetic acid. This was confirmed by the melting point of 157.3-157.9 ◦C. The percent yield determined at the end of the experiment was 37.83 %. The TLC analysis showed that P-Chlorophenol was less polar than P-Chlorophenoxyacetic Acid because it had an Rf value of 0.38 in comparison to the value of 0.33 on a 50:50 hexane and ethyl acetate solvent mixture. In the NMR comparison, it was shown that both the starting material of chloroacetic acid and product contained a peak of integration two around 4 ppm representing the acidic proton. In the FT-IR comparison, it was determined that the Chloroacetic acid and the para-Chlorophenoxyacetic acid both had an OH bond at 3416 cm-1 and 3429.72 cm-1 respectively. The Chloroacetic acid and para-Chlorophenoxyacetic acid also both had a carbon-oxygen double bond at 1648 cm-1 and 1654.81 cm-1 respectively. The para-Chlorophenoxyacetic acid also contained a peak at 1236.18 cm-1 which represents the C-O-C bond.

Table 1: Properties of the reagents and possible products for the reaction. The boiling point of Phosphoric acid is not important because it is a reagent.

The purpose of this experiment was to synthesize isopentyl acetate via an esterification reaction between acetic acid and isopentyl alcohol, using concentrated sulfuric acid as a catalyst. The product was washed with sodium hydrogen carbonate, as well as with water, then dried with anhydrous sodium sulfate. The product was then distilled using a Hickman still and characterized using infrared spectroscopy. The percent yield of isopentyl acetate was 61.52%. This may have been low due to not all of the condensed product being removed from the Hickman still, some product being lost during transfer of the product from the reaction tube into the Hickman still, or the loss of some product due to evaporation during distillation.

In this experiment, the main objective was to synthesize a ketone from borneol via an oxidation reaction and secondly, to produce a secondary alcohol from camphor via a reduction reaction. Therefore, the hypothesis of this lab is that camphor will be produced in the oxidation reaction and isoborneol will be the product of the reduction reaction because of steric hindrance. For the oxidation step, a reflux will be done and then a microscale reflux for the reduction step. The products will be confirmed using Infrared spectroscopy, the chromic acid test, 2,4-DNP test and 13C NMR spectroscopy. The results of this

In this experiment, an unknown alcohol underwent a Fischer Esterification reaction by reacting it with acetic acid as well as sulfuric acid catalyst. The unknown product material was purified through distillation and characterized by analyzing an IR spectrum and determining the density of the product. In addition, the boiling point test was performed to test for an ester. Lastly, the starting material, an unknown alcohol, was determined after finding out the product and examining the IR spectrum for the reactant.

Abstract: The purpose of this experiment is to take methyl salicylate (wintergreen oil) and by heating it under reflux with NaOH as a solvent, and then cooling the mixture with H2SO4 as another solvent, synthesize salicylic acid. The final step involves purify the product to produce as pure a sample of salicylic acid as possible. This process allowed for the successful production of 1.406g salicylic acid, an 82.70% yield. The NMR and IR both produced images that correlate with the known spectrums indicating a pure product. The melting point range was slightly wider, though did encompass the accepted melting point values.

The products of interest within this experiment are 2-methyl-1-butene and 2-methyl-2-butene from sulfuric acid and phosphoric acid catalyzed dehydration of 2-methyl-2-butanol. The reaction mixture was then separated into its separate alkene components by steam distillation and then analyzed by gas chromatography (GC), Infrared Radiation (IR) spectroscopy, and Nuclear Magnetic Resonance (NMR) imaging. Gas chromatography is an analytical technique that is able to characterize if specific compounds exist in a reaction mixture, even if they are in low quantities, assess how much of a compound exists within a reaction mixture relative to other components within the sample, and determine the purity of an isolated product. In the case of this experiment, gas chromatography is used to analyze how pure the alkene reaction sample was and if any remnants of impurities or 2-methyl-2-butanol remained in the sample after isolation of alkene components.

The purpose of this experiment is to prepare isopentyl acetate by direct esterification of acetic acid with isopentyl alcohol. After refluxing there is an isolation procedure where excess acetic acid and remaining isopentyl alcohol are easily removed by extraction with sodium bicarbonate and water. The ester is then purified by simple distillation and the IR is then obtained.

For this experiment, Alcohol D and Acid 2 reacted in the presence of concentrated sulfuric acid, resulting in a colorless solution with brown layer on top. After washes with sodium bicarbonate and brine, the pale-yellow liquid product was dried and then distilled. Distillation resulted in two colorless fractions, the second of which had a boiling point of 69-70 ˚C. This boiling point is unrealistic for any compound obtained in this experiment, so it was not used in identifying the product. After distillation, both fractions were spectroscopically analyzed. The IR and NMR spectra obtained for both fraction were identical, meaning both fractions contained exactly the same substance. Both fractions also smelled the same, like piña colada, therefore confirming this conclusion. This outcome also meant that the amount of product synthesized was 5.7393 g.

In this experiment, methyl benzoate was synthesized from benzoic acid and methanol with acid catalyze using Fisher Esterification. First benzoic acid and methanol were mixed in 100 mL round bottom flask. We cooled the mixture in ice and poured 3 mL of conc. H2SO4 and swirled to mix compounds. Then we refluxed the mixture for 1 hour. We let the solution cool and then decanted into a separatory funnel containing 50 mL of water and rinsed the round bottom flask with 35 mL of tert-butyl methyl ether and added that to a separatory funnel. We shook and vented thoroughly and drained the aqueous layer which contained a bulk of methanol and H2SO4. We washed the solution in the separatory funnel with 25 mL of water, followed by 25 mL of sat. sodium bicarbonate

Purpose: The purpose of the experiment was to perform the acid-catalyzed Fischer Esterification of acetic acid and isopentyl alcohol to form isopentyl acetate, or banana oil, which is used in flavor industries. The equilibrium of the reaction was changed by adding an excess amount of acetic acid. The reaction was refluxed and product was purified by extraction and distillation. Isopentyl acetate was analyzed by infrared spectroscopy and 1H NMR spectroscopy.

In this laboratory project, Compound “E” was identified as N-Phenylsuccinimide. The % yield was 60.5 %. The melting point of both Compound “E” and N-Phenylsuccinimide was 153-154 ⁰C, as verified through experimentation; the official melting point range of N-Phenylsuccinimide is 153-157 ⁰C. The yield of dibromobenzene was 1 gram, and the % yield of dibromobenzene was 69.2%. The purpose of this experiment was to purify an impure compound through recrystallization, and then identify it through measuring the melting point.

Carboxylic acids (Lactic, propionic, caproic, acetic, picolinic etc.) are chemicals extensively used in pharmaceutical, food and other allied industries, as they find diverse application as reactants, solvents and even as catalysts in a few work instances (Talnikar et al., 2014). These acids when obtained by fermentation of sugars, the presence of fermentation by-products, media impurities & additives like antifoam agents interfere in purification process (Pursell et al., 2009). During fermentation acids are produced essentially as mixture and mostly dilute solutions are obtained. Moreover during hetero-fermentation the broth contains mixture of acids as final product (Abdel-Rahman et al., 2013).

The experimental design of this research can be divided into five main stages. The first stage is development of yeast cell colony on nutrient agar and inoculum preparation of Candida rugosa ATCC 14830. The microorganism used in this research is isolated from natural soil. Second stage is extraction of lipase enzyme from the growth medium that contain olive oil that act as a substrate. Third stage of this project is preparation of immobilized and free enzyme culture system. The immobilized enzyme culture system is prepared with Ramsay medium as fermentation medium and calcium alginate gel beads as immobilized support. The next stage is data analysis on lipase activity on both culture systems. Finally the fifth stage is the comparison on efficiency between immobilized and free lipase culture system. The flow chart of experimental design is shown in Figure 4.1.