The lab begins with reflux of the reaction to form an ester followed by several extractions from an organic layer. To purify the ester the compound is dried by gravity filtration with a drying agent, distilled using simple distillation, and recrystallized. The aldol condensation is reacted in a test tube and the solute is collected via vacuum filtration and recrystallized. The esterification procedure was performed first. To begin the lab, the heating mantle was set at the 6 setting, and the hot plate heat was turned on to low. In a round bottom flask, 6.1 g of benzoic acid and 21 mL of MeOH were added into the flask. Once this was added to the flask, 2 mL of sulfuric acid was added and poured carefully down the side of the flask. It was noted that after the addition of the sulfuric acid there was heat production in the flask. The contents were swirled and a boiling chip was added into the flask. The flask was connected to the hood by a clamp. Water was then ran through the condenser and connected to the round bottom flask to begin refluxing the contents in the flask. The mixture was gently heated at reflux for one hour. While the esterification reaction was under reflux, the aldol condensation procedure was performed. The hot plate was turned to The washes needed to be performed and during this lab it was important to make sure that no aqueous layer remained in the organic layer. This is important for when the final product is distilled in an air tight condenser (with no water flow). The temperature would have gotten fairly high that the water either would’ve distilled out before the final product or would have caused the glassware to break due to temperature difference occurring in the setup. A better yield could have been achieved during the drying of the product, which facilitated some loss of product if there would have been some aqueous layer remaining in the organic
barbier reaction: In a 50 mL round bottom flask that had a reflux condenser attachment, saturated ammonium chloride (5 mL), THF (1 mL), zinc powder (0.4 g), benzaldehyde (0.500 mL, 0.5225 g, 4.92 mmol), and allyl bromide (0.470 mL, 0.6533 g, 5.40 mmol) were charged with stir bar and stirred at room temperature for 45 minutes. Diethyl ether (10 mL) was added to the reaction mixture and stirred. The mixture was gravity filtered into a beaker that was topped with a watchglass. The filtrate was transferred to a separatory funnel and the organic layer was extracted with deionized water (10 mL) and diethyl ether (15 mL). The organic layer was placed into an Erlenmeyer flask and the aqueous layer was placed into a beaker, which was extracted with
need is water and an ester and we will end up with an organic acid produced as
Procedure: A sand bath was set atop a hot plate set at power level 5, while a 10 mL round bottom was prepared with the addition of 14 (0.33 mL) drops of olive oil and 1 mL of cyclohexene. Once the contents of the 10 mL round bottom were mixed thoroughly, a boiling chip was added, and the round bottom was attached to a reflux condenser apparatus. The reflux was run for 20 minutes starting at the point in time when the mixture within the round bottom flask (that was submerged in the heated sand bath) began to boil. While the running the reflux, a 5 ¾ inch Pasteur pipette was obtained and clamped vertically with the tip facing downward. A small amount of glass wool was placed inside of the pipette and pushed down to block the narrowing end by a wooden boiling stick. A total of 100 mg (0.100 g) of celite was weighed out and was carefully added into the pipette as an additional layer atop the glass wool stopper.
The three butene products have been verified to elute in the following order: 1-butene, trans-2-butene, and cis-2-butene. Theory: The dehydration of 2-butanol, a secondary alcohol, progresses readily in the presence of a strong acid like concentrated sulfuric acid (H2SO4). The reaction is completed via the E1 mechanism. Initially, the hydroxyl group is a poor leaving group, but that is remedied by its protonation by the acid catalyst (H2SO4) converting it to a better leaving group, H2O. The loss of this water molecule results in a secondary carbocation intermediate that continues to form an alkene in an E1 elimination.
In step one, a 0.1 grams of 4-t-butylcyclohexanone and 0.2 mL of methanol was placed into a long-neck round-bottom flask. The contents were swirled and a boiling chip was placed. 0.023 grams of NaBH4 was weighed to prepare the sodium borohydride solution. Once ready, 0.6 mL of the sodium borohydride solution was added to the apparatus. The reaction was allowed to proceed for about ten minutes. During this time, 0.5 mL of 1 N HCL was chilled in a small dram vial. Once the reaction was complete, using a pipette the cold hydrochloric acid was added to the flask. In step nine, the solution was extracted three times using 0.5 mL increments of methylene chloride. To do this the contents from the flask were washed with one 0.5 mL increment
Ø Then pour the catalyst into a test tube along with the H O and
Ensure gloves are worn at all times when handling strong acids and bases within the experiment of the preparation of benzocaine. 4-aminobenzoic acid (3.0g, 0.022 moles) was suspended into a dry round-bottomed flask (100cm3) followed by methylated sprits (20 cm3). Taking extra care the concentrated sulphuric acid of (3.0 cm3, 0.031 moles) was added. Immediately after the condenser was fitted on, and the components in the flask were swirled gently to mix components. It should be ensured that the reactants of the concentrated sulphuric acid and the 4-aminobenzoic acid were not clustered in the ground glass joint between the condenser itself and the flask. In order to heat the mixture to a boiling point, a heating mantle was used and then further left for gently refluxing for a constituent time of forty minutes. After the duration of the consistent forty minutes the rou...
As a final point, the unknown secondary alcohol α-methyl-2-naphthalenemethanol had the R-configuration since it reacted the fastest with S-HBTM and much slower with R-HBTM. TLC was a qualitative method and ImageJ served as a quantitative method for determining which reaction was the faster esterification. Finally, 1H NMR assisted in identifying the unknown from a finite list of possible alcohols by labeling the hydrogens to the corresponding peaks.
To start this study, nine labeled test tubes were setup with precise amounts of 2mL of deionized water, and 1ml of 50-50 corn syrup to water mixture. The addition of 1mL of yeast would also be added, but this will not be added until the fermentation apparatus is assembled in the water bath and ready to begin the reaction. The assemble of our apparatus included submerging and combining of the test tube and tubing with a stopper to ensure no air is in the apparatus. Then the assemble would be put this apparatus with water inside a Styrofoam cup, to ensure temperature is conserved best, and prepare to add the test tube with controlled substance to the test tube and stopper. The water baths at different temperatures are the only variables changed. One water bath was set up as the control group at room temperature, 28°C. The second water bath was setup to 0.4°C by use of ice water, and third bath used hot water at 49°C. Right before adding the test tube with control substance, the yeast would be added to create the reaction that produced the gas. To ensure best accuracy of fermentation, an initial test tube with all substances but yeast was performed to obtain an initial equilibrium time. Measuring of this time occurs till no more air is bubbling out of tube. This time is where we would mark are initial measuring line for each of the following reactions. As the gas pushes the water out of the test tube
For this experiment we have to use physical methods to separate the reaction mixture from the liquid. The physical methods that were used are filtration and evaporation. Filtration is the separation of a solid from a liquid by passing the liquid through a porous material, such as filter paper. Evaporation is when you place the residue and the damp filter paper into a drying oven to draw moisture from it by heating it and leaving only the dry solid portion behind (Lab Guide pg. 33.).
In a 100ml beaker place 50mls of water, measure the temperature of the water and record this initial temperature onto a table. Set the timer and add one teaspoon of Ammonium Nitrate to the water, stir this continuously until the Ammonium Nitrate has dissolved.
The aim of this experiment was to investigate the affect of the use of a catalyst and temperature on the rate of reaction while keeping all the other factors that affect the reaction rate constant.
The solvent should be easily removed from the purified product, not react with the target substances, and should only dissolve the target substance near it’s boiling point, but none at freezing. A successful recrystallization uses minimum amount of solvent, and cools the solution slowly, if done to fast, many impurities will be left in the crystals. Using the correct solvent, in this case ice water and ethyl acetate, the impurities in the compound can be dissolved to obtain just the pure compound. A mixed solvent was used to control the solubility of the product. The product is soluble in ethanol an insoluble in water. Adding water reduced solubility and saturates the solution and then the crystals
After performing the first Gas Chromatography, we took the organic layer, and mixed it with saturated Sodium Hydroxide. We performed this step to remove the (-OH) group from the Eugenol. The purpose was to make the water as a product, which can also be used as a solvent for the Eugenol that was ionized, for the two substances Acetyl Eugenol and Beta Caryophyllene. Again, we see the density differences in the solvents; we were able to take the organic layer. Finally, we transferred the layer into the beaker and dried, to perform the Gas Chromatography
The catalytic process occurs at lower temperature anf offers higher selectivity but requires frequent regeneration of the catalyst. Then, the products are cooled and introduced into a pair of separators which separate the unreacted hydrogen. The unreacted hydrogen is compressed and recycle back to the feed and reactor. The products that leaving the separators are heated before introduced into a distillation column which the toluene is separated from the stream and recycle back to the...