Β-D-Pentaacetate Synthesis

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

There are millions of different organic compounds. Most of them are found in mixtures and in order to achieve a pure form they need to be separated, isolated, and purified. However, there are endless numbers of possible mixtures, which make it impossible to have a pre-designed procedure for every mixture. So chemists often have to make their own procedures. The purpose of this experiment was to prepare the student to the real world by them designing their own procedure which will help them understand the techniques of separation and purification better. The goal was to extract two of the components of the

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

Experiment 55 consists of devising a separation and purification scheme for a three component mixture. The overall objective is to isolate in pure form two of the three compounds. This was done using extraction, solubility, crystallization and vacuum filtration. The experiment was carried out two times, both of which were successful.

Abstract: One mixture of two unknown liquid compounds and one mixture of two unknown solid compounds were separated, isolated, purified, and characterized by boiling point. Two liquid unknowns were separated, isolated, and purified via simple distillation. Then, the process of an acid-base extraction and washing were used to separate two unknown compounds into two crude compounds: an organic acid and a neutral organic compound. Each crude compound was purified by recrystallization, resulting in a carboxylic acid (RCO2H) and a pure organic compound (RZ). The resulting mass of the pure carboxylic acid was 1.688g with a percent recovery of 31.80%, the boiling range was 244-245 °C, and its density was 2.0879g/mL. The resulting mass of the pure organic solid was 2.4902g with a percent recovery of 46.91%, the boiling range was 52.0-53.4°C, and its density was 1.5956 g/mL.

The reaction took place in a conical vial and .2mL of each of the reactant samples were added to it along with some 95% ethanol. Two drops of NaOH were added shortly after and stirred at room temperature for fifteen minutes. The vial was cooled in and ice bath and crystallized. Vacuum filtration was performed to filter the crude product. The crude product was recrystallized using methanol and filtered again. We made one change to the procedure and instead of using .7mL of ethanol we

An ester was synthesized during an organic reaction and identified by IR spectroscopy and boiling point. Acetic acid was added to 4-methyl-2-pentanol, which was catalyzed by sulfuric acid. This produced the desired ester and water. After the ester was isolated a percent yield of 55.1% was calculated from the 0.872 g of ester recovered. This quantitative error was most likely due to product getting stuck in the apparatus. The boiling point of the ester was 143° C, only one degree off from the theoretical boiling point of the ester 1,3-dimethylbutyl, 144 ° C. The values of the

Based on prior calculations, expected yield for the alkene products was 79.5%. The actual yield was not as high, resulting in a 28.4% yield. Even with this relatively small yield, the reaction still went to completion as indicated by the GC results in Figure 2. This is known because there is no presence of 2-methyl-1-butanol within the GC spectra. Only the two desired alkene products with

Part 2 to determine the empirical formula and percentage yield of the compound synthesized in Part 1. Spectrophotometry is a routine laboratory test that has the added advantage

Electrophoresis of the purified enzyme was done to determine its molecular weight and some properties of the purified enzyme were

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 synthesis of the product: β-D-glucose pentaacetate is done though the acetylation using acetic anhydride with D-glucose with the help of sodium acetate. The recrystallization of the product is done though a polar solvent like water. The Result of this experiment has a percentage yield of 61% and analytical methods that are to detect the products are 1H NMR, 13 C NMR, COSY, FTIR (IR), Thin Layer Chromatography (TLC) and Melting point.

Step 1 and 2 was repeated by using distilled water by replacing the test solution.

There is no need of purification in this method as there is no residual solvent obtained in this method.

As shown in table no 1, the percentage yield of methanolic extract of L. inermis is 17% while recovery yield of Hexane, ethyl acetate and methanol fractions are 4%, 5.7% and 70%, respectively. It indicates that approximately 20% was lost during the fractionation. Kawo and Kwa 57 reported 1.8% ethyl acetate fraction yield which is lower than our report while recovery yield of aq. methanolic fractions is higher (87.19%) than our reported value.