Isolation Of Betulin From Bich Barks

The dehydration of 2-methyl-2-butanol was performed using sulfuric acid and phosphoric acid in order to synthesize alkene products 2-methyl-1-butene and 2-methyl-2-butene. After carrying out steam distillation to isolate the organic alkenes from aqueous components within the reaction mixture, the purity and characterization of the products were then assessed through various analytical methods including Gas Chromatography (GC), Infrared Radiation (IR) Spectroscopy, and Nuclear Magnetic Resonance (NMR) Imaging. Through the characterization of the final products, it was found that little impurities remained in the final reaction solution and according to the GC, no alcohol remained in the vial after the reaction was complete. The actual yield

The product ratio of N-ethylsaccharin to O-ethylsaccharin that occurred due to alkylation with iodoethane at 80 oC was determined to be 81.5% to 18.5%, respectively, based on an analysis of the 1H NMR spectrum that was collected. The melting point range of 87.8-94.7 oC also indicated that the mixture was largely composed of N-ethylsaccharin. The more prevalent product structure is:

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 light yellow precipitate was collected by suction filtration using a Hirsch funnel. The product was washed with two 1-mL portions of cold methanol followed by two 1-mL portions of diethyl ether. The product was dried in the oven at 110°C. The IR spectrum as a KBr pellet was obtained for the product and inosine for analysis.

The extraction of the p-tert-butylphenol was then carried out in the exact same fashion as the p-toulic acid, with the exception that the aqueous solution added to the remaining ether solution was 10 mL of 0.5M NaOH. The solution was mixed and the gas was in the funnel, along with the extraction of the aqueous layer three times into a clean and labeled 100-mL beaker. As in the previous step an addition of 5 mL of deionized water was used in the final extraction step. The extracted solution was also saved for later in the experiment as was the ether layer remaining in the separatory funnel.

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.

The objective of this experiment is to successfully perform a dehydration of 1-butanol and 2-butanol, also dehydrobromination of 1-bromobutane and 2-bromobutane to form the alkene products 1-butene, trans-2-butene, and cis-2-butene. The dehydration reactions react under and acid-catalysis which follows an E1 mechanism. It was found that dehydration of 1-butanol yielded 3.84% cis-2-butene, 81.83% trans-2-butene, and 14.33% 1-butene, while 2-butanol is unknown due to mechanical issues with the GC machine. For the dehydrobromination, with the addition of a

On a thin chromatography plate, five spots were placed ( as shown in table 2) and the plate was developed using chloroform/methanol. This was later visualized with dragendorff’s reagent under the UV light. All separated components were observed, identified and recorded.

A calibrated pipette was used to measure 0.655mL (5.4 mmols) of p-tolualdehyde into a preweighed 10 mL graduated cylinder, and the graduated cylinder was reweighed to obtain the mass of the p-tolualdehyde. The aldehyde was dissolved in 2 mL of methanol and stirred. The solution was added to the ylide solution in the 100 mL round-bottom flask. The flask was placed into a reflux apparatus and refloxed for 15 minutes. The solution was added to the separatory funnel after reflux and 15 mL of water was added and mixed. Two aqueous layer was extracted with two portion of 15 mL of hexane. The hexane extracts where were combine and a drying agent was added to remove residual aqueous solution. The dried hexane was decanted into a prewieghed round bottom flask and placed into the rotary evaporator. The flask was reweighed to determine the yield (0.717g). A NMR sample was prepared by adding 5 drops of CDCl3 to your product and mix well. To the NMR tube one drop of the resulting solution and 0.50 mL of CDCl3 was added, capped and given to the instructor to be analyzed by

A development chamber was also set up with filter paper and 70% hexane -30% acetone as the solvent. This solvent was also used to dissolve the dried pigments, which were then spotted onto the TLC plate. The TLC plate was then placed into the development chamber and removed once the solvent traveled near the top. Image 1 shows the TLC plate after this experiment. Each of the pigments could be identified for each spot on the TLC plate. The top pigments that are yellow-orange are the carotenes; they are indicated under the extract and yellow band spots. In decreasing order from top to bottom, the spots are carotenes, pheophytin a, pheophytin b, chlorophyll a, chlorophyll b, and xanthophylls. Xanthophylls are yellow spots and are the last three spots towards the bottom of the plate. For the green band, there were no yellow spots and the green spots have the most color; this most likely proven that the green band are the chlorophyll pigments. However, almost all of the colors on the plate were not as intense as they should be; the pigments were spotted as small dots and thus, less concentration of each pigment interacted with the solvent. While performing thin-layer chromatography though, a possible error might have occurred, which was adding a little too much solvent in the development chamber. When the TLC plate was placed into the chamber, the solvent was above the line where the pigment spots were located. Nevertheless, all of the pigments in the carotenoids and chlorophylls were distinguishable on the plate. Data Table 1 shows the Rf value for each pigment spot, including the

This paper mainly deals with a small family of proteins ‘Lipocalins’. The structures and functions of different lipocalins have been widely discussed. The structural similarity, physiological functions, synthesis, their number of amino acid residues, secondary structures of each lipocalin has been widely analyzed throughout this paper.

Diluted essence (10ml, 100 times diluted) was pipetted into a 100ml separating funnel. 20ml of dichloromethane was added to the diluted essence. The funnel was then shaken vigorously for 2 minutes with gas being release occasionally. The organic phase (lower layer) was released into a 100ml beaker and another 20 ml of dichloromethane was added to the funnel and shaken vigorously for another 2 minutes. The organic phase (lower layer) was again released into the 100 ml beaker. The contents of the funnel were disposed of. The organic phase was then added back into the separating funnel with 40ml of 0.1M sodium hydroxide solution and shaken well for 2 minutes. The organic phase was released and disposed of and the aqueous phase was kept and transferred to a 250ml volumetric flask and the volume was made up with 0.1M sodium hydroxide. Standards were then made using the 50mg/L standard provided and mixing with 0.1M sodium hydroxide to create standards with 1,2,3,4,5 mg/L concentrations. Each solution was run through the UV – Visible spectrometer to find the absorbance and then the concentration.

Methodology: Using auto-pipette (20-100 microlitre), pipetted 0.06 mg of Taxifolin was added to 10ml conical flask and made up to the mark (10ml) with H2O.This procedure was repeated with the same amounts foe silymarin stock solution and silybum marianum extract. Taxifolin was transferred to 2ml brown bottle for HPLC auto sampler, this was also done to silymarin stock solution. Silybum marianum extract was filtered via a syringe filter (0.2 microlitre).The three

During this experiment the crude product (mixture of ortho and para nitrophenols) was run through a column chromatography. The point of the column chromatography was to separate the nitrophenols and purify them. During the experiment the crude product was ran through the silica with two different solvents. 60:40 DCM/hexanes was used to form the first band while 50:50 DCM/EtOAc was used to form the second band. The reason for this method was that there had to be a change in solvent for the para product because since it is polar it was expected to run very slowly through the column and therefore needed a more polar solvent to speed it up, ethyl acetate. As expected two different yellow bands were observed. Each band represented one of the nitrophenols, with the bottom band being the ortho-nitrophenol since it is less polar and stayed within the solvent and therefore ran through the column quickly. The para product stayed at the top because it was similarly polar to the Silica and had the ability to hydrogen bond to it. Once the bands were formed fractions were taken from the yellow bands. Fraction 1-5 was from the ortho product and fractions 6-10 were from the para product. The fractions formed were than ran through TLC chromatography to test the true purity of the products and the success of the column chromatography separation. The first TLC plate containing fractions 1-5, surprisingly did not have any spots (Figure 1b). This is was unexpected because fractions 1-5 were

In the proposed method, the sample solution is dissolved in acetonitrile with (1 mg/mL of an analog of fentanyl (CH2CH2CH2) as an internal standard) so that the sample solution is at a concentration of 0.1mg/mL. 1mL of the acetonitrile solution is placed into a centrifuge with 50mg of 4-DMAP (4-(dimethylamino)-pyridine) and 50microL of HFBA (heptafluorobutyric anhydride). The solution is allowed to react for 1h at 75C, following which 5 mL of isooctane and 1N of aqueous sodium carbonate are added, and then centrifuged. 1 mL of this layer is then diluted using 10 mL isooctane. 5 mL of this dilution is placed in a centrifuge tube and back extracted using 5mL of 1 N sulfuric acid. The solution is then ready to be chromatographed. If the sample solution is adulterated with sugars, prior to dissolving the solution in acetonitrile, dissolve an amount equivalent to .1 mg of fentanyl in