The yellow solution containing the reactants was slowly poured into the beaker containing the cold water and the acid in order to cause the precipitation of the alcohol, 9-fluorenol and to destroy (hydrolyzed) the unreacted excess sodium borohydride. Subsequently, the white precipitate was vacuum filtered and washed twice with 20.0 ml portions of distilled cold water by pouring the liquid into the Buchner Funnel during filtration. It was necessary to wash the alcohol prior to recrystallization considering that the C-OH bond is easily broken by the formation of a stable and benzylic carbocation that favors the synthesis of difluorenyl ether. Finally, before the purification by recrystallization of the obtained product, the white solid alcohol was allowed to dry over a period of a
After recrystallization and purification, the percent yield was 63.620% (0.724 grams) and the melting point was 262-263°C (see Table 1). The literature melting is 262-264°C. The low percent yield could be due to lack of recrystallization of the crude product. In addition, some of the crystals may not have been transferred to the funnel from the flask.
In this laboratory experiment, 3.030 g of Isopentyl Acetate was synthesized and formed by the esterification of acetic acid with Isopentyl Alcohol. 1.0 mL of Sulfuric acid was used as a catalyst in the reaction. The excess Isopentyl Acetate was used to shift the reaction to the right for esterification to occur. During the extraction, the excess of acetic acid and Isopentyl alcohol was extracted with sodium bicarbonate, and further purification of the Isopentyl acetate was done after through drying with anhydrous sodium sulfate and through simple distillation. The percent yield of the Isopentyl Acetate was 46.6 percent with a theoretical yield of 6.502g. In this laboratory experiment the acetic acid was in excess and the Isopentyl Alcohol was the limiting reagent,
Although 3 pentanol is polar with an alcohol group attached to its end, its hydrocarbon chain decreases its solubility in water, making it possess a lower affinity for the stationary phase and elute first. In the second fraction, only one main peak could be identified at 3265.26 cm-1 that matched the provided IR spectra. This peak represents another alcohol group which limits it down to 3-methyl-butanol, 2 heptanol, 2 octanol, and 1 hexanol. Since this was the second fraction, it must be more polar than the first fraction to elute last. Therefore, by elimination, the second fraction was identified as 3-methyl-butanol.
Because the heating block readily increased in temperature, the temperature had to be adjusted accordingly to prevent the overheating the reaction. Initially, the color of the reaction turned into a dark green color and over time became a lighter shade with a minimal solid left. The reaction process lasted for 2 hours. As the reaction heated for 2 hours, a 50 mL beaker was weighed, approximately 12 mL of 20% ethyl acetate in hexane solution was added to a 25 mL Erlenmeyer flask, and 2.0 mL of saturated NaCl solution was added to a labeled test
Approximately 10mg of the white crystalline product was dissolved in 0.5mL of 95% ethanol in a small test tube to make a colorless solution. 10. The product was then introduced to 0.5mL of 2% ethanolic silver nitrate for the silver nitrate test. 11. The silver nitrate was let to stand for 5 minutes with the product and ethanol.
Abstract: The purpose of this experiment was to identify given Unknown White Compound by conducting various test and learning how to use lab techniques. Tests that are used during this experiment were a flame test, ion test, pH test, and conductivity test. The results drawn from these tests confirmed the identity of the Unknown White Compound to be sodium acetate (NaC2H3O2) because there were no presence of ions and sodium has a strong persistent orange color. The compound then will be synthesized with the compounds Na2CO3 and HC2H3O2 to find percent yield.
In this oxidation benzoin to benzil experiment, students placed 1.0g of benzoin from the previous lab with 0.50g of ammonium nitrate in round bottom flask. Nitrate in ammonium nitrate can regenerate from Cu+ to Cu2+ after finished first oxidized benzoin. Then, add 4.0ml of glacial acetic acid and 1.0ml of 2% cupric acetate as
Each solution was put in separate labeled test tubes. Original observations were recorded. 6M NaOH was added until a precipitate was formed (20 drops were not exceeded). Observations were then recorded into the lab manual. To the solutions that created a precipitate and addition of ten drops of NaOH was added.
Then 200 µl of the solution phenol/chloroform/isoamyl alcohol (25:24:1) was added to the tubes under the fume hood and tubes were placed on rotator and left to mix for 3 min. 200 µl of TE buffer was added and spun for 5 min at maximum speed, the water phase was transferred to new tubes. 1 ml of cold 96 % ethanol was added, mixed and then spun for 5 min at maximum speed at 4°C. the supernatant was discarded and the pellet re-suspended in 400 µl of TE buffer (40 mM Tris-Base, 20 mM acetic acid, 1 mM EDTA, pH 8.0). 6 µl of 7.5 M ammonium acetate was added and the pervious step was repeated.
Physical observations sodium benzoate 2.15 1.3 White powder; clumps up easily Once the crude product had dried completely, the melting point was taken. Sodium benzoate and benzoic acid had extremely different melting points so it was simple to determine what the final product was (Figure 4). The final product had corrected melting point ranges that accurately matched benzoic acid (Figure 5).
The problem at hand is that the reaction kinetics is not known and need to be determined to understand the reaction more thoroughly. There is a hypothesis that the reaction kinetics is exactly the same for different types of reactors. The purpose of
CHAPTER 4 SUMMARY OF RESULTS, CONCLUSION AND RECOMMENDATIONS Summary As the researchers completed the process of making the product which undergone extractions and pre-treatment, different tests we’re conducted in terms of physical and chemical properties in relation to the commercial ethanol. For the physical properties of BIT and commercial ethanol, the ethanol showed different measurements in physical properties of BIT and commercial ethanol such as the density, smoke emission, and heat. Based on the given data, BIT and commercial ethanol are close to each other in terms of density and smoke emission.