To a magnetically stirred solution of 3-methylcyclopentene-1,2-dione 1 (1 mmol) and N-isocyaniminotriphenylphosphorane 3 (1 mmol) in CH2Cl2 (10 mL) was added dropwise a solution of dimethyl acetylenedicarboxylate 2 (1 mol%) in CH2Cl2 (5 mL) at –10◦C over 15 min (Scheme 1). The mixture was stirred for 2 h at room temperature. The reaction mixture was stirred at the same conditions (–10◦C) for 2 h, and then the mixture was allowed to warm up to room temperature and was stirred for 4 days. The solvent was removed under reduced pressure and the viscous residue was purified by flash column chromatography (silica gel powder; petroleum ether–ethyl acetate, 10:1). The solvent was removed under reduced pressure and the product 4 was obtained. The characterization
can be used to aid Narcolepsy. It was first discovered during the search for an cure for
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
0.152 grams of p-aminophenol was combined with Exactly 0.5 mL of water and 0.3 mL of acetic acid. A magnetic spin vane and a magnetic stirrer on the hot plate was used to reflux the reactants. The heat was necessary to break down the covalent bonds in p-aminophenol and polarity of water was essential to create acetaminophen. Originally, the experiment did not turn as planned because the temperature was set above 100 ℃ and the solution was evaporated. The experiment was conducted again with another group. The vial was then placed in an ice bath while before it was poured down the Hirsch funnel and rinse the vial with 0.5 mL of cold to the pour the remaining crystals into the
The mixture was then placed into a separatory funnel that we had set up. Petroleum ether was used to rinse the solution in the reaction flask. 20ml of saturated sodium chloride were added to the separatory funnel and was shake. The petroleum ether layer was drained into a flask and was dried with anhydrous sodium sulfate. The solution was the filtered by gravity filtration. 1ml of the petroleum ether filtrate was transferred to a 3ml vial. 5 drops of 5% methyl heptadecanoate in chloroform was then added to the vial and mixed. GC analysis was then preformed.
Residual solvents are defined as organic volatile impurities that may remain in active Pharmaceutical substances, excipient or medicinal products after processing. During the manufacturing processes, the solvents are not completely removed. The solvents may be used to improve the yield in the synthesis of active pharmaceutical substances besides imparting characteristics of crystal form, purity and solubility. Residual solvents do not have any therapeutic effect. Therefore, efforts should be made to remove them to the extent possible to meet the specification prescribed [2]. Gas chromatography method has been developed to find out the purity of acetone, dichloromethane, methanol and toluene. Using this technique, the major contaminants of each
The product of interests was able to eventually be separated due to extraction and washing using a separatory funnel and later short path distillation. The addition of water and diethyl ether allowed for the extraction of 1-ethoxybutane into the organic ether layer, and the sodium and bromide ions into the aqueous water layer. This was evident by the disappearance of the precipitate, because sodium bromide dissociated in water into its cation and anion components. In other words, the addition of water quenched the reaction and allowed for no other reaction to take place. 1-ethoxybutane remained in the ether layer because it was mostly nonpolar. The organic layer was on the top, and the aqueous layer was on the bottom due to the heavier weight supplied by the bromide ion of sodium bromide.
The purpose of this experiment is to analyze mixtures of compounds prior to, during and after a separation scheme. This experiment also allows monitoring reactions of organic molecules, and determines the identity of a mixture of compounds.
The mixture was heated to a gentle boil and then the distillation was allowed to begin. The heat was turned off after the temperature of the steam stayed constant. The distillation continued until approximately 40 mL of the liquid was obtained. The 40 mL of distillate was transferred to a 250 mL separatory funnel. A small amount of dichloromethane was used to wash the receiver after the transferal. The distillate was extracted with 10 mL of dichloromethane three times, each time using a little extra dichlormethane to wash each layer. The organic layer on the bottom was collected for each extraction. All organic layers were collected in a 125 mL Erlenmeyer flask. Anhydrous sodium sulfate was used to dry the solution for fifteen minutes. Meanwhile, a vacuum filtration apparatus was set up accordingly. A 250 mL filter flask was obtained and pre-weighed. The solution containing the limonene was vacuum filtrated while it was kept warm in a steam bath. Additional Sodium Sulfate was added to the solution to remove excess water. The solution was then washed 3-4 times with dichloromethane and the vacuum filtration continued. The vacuum pump was turned off when the flask contained only a small amount of oil. The flask was then weighed.
After completion of the transesterification reaction employed at the optimal conditions, the catalyst was collected from the reactant mixture by filtration; the catalyst was washed with hexane several times to remove the adhered oil particles, and then dried at 110°C for 2 hr. The catalyst was reused several times without further treatment to obtain FAME from WCSO.
In part one of the experiment, Flourene (0.1 g, 0.0006 mole) was measured and added to a 25 mL Erlenmeyer flask. Next, 10 M of NaOH (7 mL, 0.2 mole) was added to the flask with a ½ inch stir bar. The mixture was stirred until the fluorene dissolved completely. Then, Stark’s Catalyst, Aliquat 336 (5 drops) was added to the solution. The color of the solution turned yellow and two layers formed. The reaction was then stirred vigorously. Next, a comparison TLC was conducted against the starting material in a 20% dichloromethane and 80% hexanes solution. The reaction stirred for 5 minutes and after that a TLC was conducted. The mixture was not complete and after another 5 minutes another TLC was conducted. Next, the reaction was poured into a separatory funnel and the organic layer was separated from the aqueous layer. Then, 5% HCl (5 mL) was added to the separatory funnel to wash the organic layer, this was repeated two more times. Next, saturated NaCl, Brine (5 mL) was added to the separatory funnel and was drained. The organic layer was then poured to an Erlenmeyer flask and Na2SO4 was added to dry it. The organic layer dried for 5 minutes then a gravity filtration was conducted to remove Na2SO4. The filtrate was collected in a pre-weighed 100 mL beaker (46.7208 g). Na2SO4 was rinsed with toluene (3 mL) twice. The beaker was labeled and placed in the hood.
Normal pentane (nC5), normal heptane (nC7), and Dodecane (nC12) (provided by Fisher Scientific) were used as the hydrocarbon solvent for extra-heavy oil recovery (dead oil viscosity = 30,000 cp at 22 °C and dead oil density = 0.933 g/cm³). Table 1 lists some of the main properties of applied solvents.
1-Vinylimidazole (VIm), 1-idobutane (IB), 2-aminoethanethiol (AET), acetylacetate, N,N'-dicyclohexylcarbodiimide (DCC), N-hydroxysuccinimide (NHS), posstasium carbonate (K2CO3), and azobisisobutyronitrile (AIBN) were purchased from Sigma-Aldrich (Milwaukee, WI, USA). 4,4′-Bis(4-hydroxylphenyl) valeic acid (HPV), 4,4′-difluorobenzophenone (DBP), chloroform, sodium hydroxide (NaOH), dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), toluene, hydrochloric acid (HCl), tetrahydrofuran (THF), iso-propanol (IPA), and dimethylformamide (DMF) were purchased from TCI company (Tokyo, Japan).
Half of the benzaldehyde- acetone mixture was added in one portion while stirring the solution vigorously. At this stage, a precipitated was formed after a few minutes. After 15 minutes, the remaining benzaldehyde- acetone mixture was added and the mixture was stirred for a further 30 minutes. After 30 minutes, the precipitate was collected by vacuum filtration and washed with cold water until the washings were
A mixture of 2a-d (0.01mol) in formic acid (99%, 30 ml) and catalytic amount of conc. H2SO4 was heated under reflux for 16 hours. Then the reaction mixture was cooled, poured into ice cold
Traditionally various chemical process are carried out to synthesis most of the commercial surfactant. Petrochemicals are being used as raw materials for production of surfactant, due to their huge availability, cost, and performance. For example some petrochemical are as follows paraffin, benzene, olefin fatty alcohol, fatty acid, and ethanol-amine, ethylene oxide, propyl-oxide etc.