The objective of this experiment was to create synthesize methyl eugenol from eugenol, dimethyl carbonate, and tetrabutylammonium bromide. To start off the experiment, a heating under reflux apparatus was used and the parts included: a water jacketed condenser, ring stand, tubes, flowing water, 25-mL round bottom flask, heating block, and a hot plate. There were two parts to the water condenser, entry and exit ways for water. The bottom opening was connected to the sink through one tube and the top opening was connected with a loose end, which was needed to get rid of the flowing water. To create the solution needed to synthesize methyl eugenol, approximately 0.200 g of eugenol (note: the measured g was converted to mg for later calculations) was measured, alongside approximately 1.2 g of TBAB and was added to the 25-mL round bottom flask. As a safety precaution, the measured 4.0 mL of DMC was added to the flask under the hood. A stir flea was then added and was used to dissolve the TBAB. After dissolving the TBAB, approximately 0.52 g of potassium carbonate was added to the flask (note: potassium carbonate is hygroscopic and could readily take in moisture). …show more content…
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
After 28 minutes, the mixture stopped boiling, and approximately 4.5 ml of bromobenzene was added drop by drop in the mixture, and color of the mixture was turned light brown orange. Then, the phenylmagnesium bromide was cooled in ice bath for a few minutes, and 10 ml of anhydrous diethyl ether was added in the mixture by using the syringe. After that, approximately 2.3 ml of methyl benzoate was added to the reaction, and it was added slowly slowly because the reaction was exothermic which needed to be cool in order to maintain a gentle reflux. Once all the methyl benzoate solution was added, the heating mantle was removed from the reaction flask and was cooled to the room temperature. During the reaction, a milky white salt began to precipitate, and the reaction flask was swirled for ten minutes until most of the reaction became visibly subdivided.
Next, about 10 mL of both solutions, Red 40 and Blue 1, were added to a small beaker. The concentration of the stock solution were recorded, 52.1 ppm for Red 40 and 16.6 ppm for Blue 1. Then, using the volumetric pipette, 5 mL of each solution was transferred into a 10 mL volumetric flask, labelled either R1 or B1. Deionized water was added into the flask using a pipette until the solution level reached a line which indicated 10 mL. A cap for the flask was inserted and the flask was invented a few times to completely mix the solution. Then, the volumetric pipette was rinsed with fresh deionized water and
A mixture of 0.25 g of camphor (1.64 mmol), 1.5 mL of methanol, and 0.25 g of sodium borohydride (6.60 mmol, NaBH4) was boiled for 2 minutes. Moreover, the addition of 10 mL of ice deionized water resulted in a white solid after the organic solution was vacuum filtered. The organic solid was dissolved in 10 mL of dichloromethane (CH2Cl2) and small amounts of anhydrous sodium sulfate (NaSO4) to dry. The organic solution was decanted and evaporated for melting point (203.3-203.8 °C), NMR, and IR spectroscopy. Product formation and heats of formation (borneol = -1.203675E6 kJ/mol, isoborneol = -1.203687E6 kJ/mol) were analyzed.
Intro: Chemical reactions are the foundation for all organisms to exist. Paragraph 1: Endergonic Anabolic Reactions Building Consumes energy to build complicated molecules from simpler ones Uphill Photosynthesis Uses water and carbon dioxide to create sugar and oxygen Protein synthesis from amino acids Dehydration reaction Monomers are covalently bonded to each other through the loss of water Bonds are created which means energy is used Endergonic Exergonic Breaking Release energy by breaking down complex molecules to simpler molecules
After obtaining an homogeneous mixture, the flask was placed in an ice bath during five minutes next to a graduated cylinder containing 5.0 mL of concentrated sulfuric acid. The temperature of the ice bath was recorded to be 1.1 °C. Likewise, a second graduated cylinder containing 1.8 mL of nitric acid and 2.5 mL of sulfuric acid was immersed in the cold ice bath to keep the three different solutions at the same temperature. Thereafter, the cold 5.0 mL of H2SO4 were added to the erlenmeyer flask containing the acetanilide solution, which remained in the cold water for approximately another 4 minutes.
Benzyne Formation and the Diels-Alder Reaction Preparation of 1,2,3,4 Tetraphenylnaphthalene Aubree Edwards Purpose: 1,2,3,4-tetraphenylnaphthalene is prepared by first producing benzyne via the unstable diazonium salt. Then tetraphenylcyclopentadienone and benzyne undergo a diels-alder reaction to create 1,2,3,4-tetraphenylnaphthalene. Reactions: Procedure: The reaction mixture was created. Tetraphenylcyclopentadienone (0.1197g, 0.3113 mmol) a black solid powder, anthranilic acid ( 0.0482g, 0.3516 mmol) a yellowish sand, and 1,2-dimethoxyethane (1.2 ml) was added to a 5-ml conical vial.
The reaction to synthesize benzocaine was known as a Fisher esterification reaction. The Fisher esterification was reaction between alcohol and carboxylic acid in the presence of acid. The reaction was used to form an ester. In the experiment, sulfuric acid acted as a catalyst and necessary for this reaction to occur. There was a change between the –OH group of carboxylic acid to an –OCH2CH3 group in the reaction.
However, after refluxing for a while, yellow precipitates begin to form near the top of the flask. It was assumed that the remaining starting material was concentrated from a decrease volume to reappeared in solution. Nevertheless, this may have been a sign of contamination that will negatively affect the entire reaction. This observation later resulted in a yellowish
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.
Discussion: 1. The Diels alder reaction has to be heated slowly to 60-70 degrees Celsius because if it is heated too quickly and the temperature gets too high the 2,3-dimethyl-1,3-butadiene will boil. A round bottom flask was attached to a water condenser to prevent any product from boiling and evaporating out during the heating process. For the hydrolysis part of the experiment the temperature needed to be 60-80 degrees Celsius to melt the cyclic anhydride but also prevent the reaction from boiling and losing product from evaporation. Lastly the final product crystals were not washed with hot water because it would have melted the crystal thus cold water was used.
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
Experiment 2 Report Scaffold (Substitution Reactions, Purification, and Identification) Purpose/Introduction 1. A Sn2 reaction was conducted; this involved benzyl bromide, sodium hydroxide, an unknown compound and ethanol through reflux technique, mel-temp recordings, recrystallization, and analysis of TLC plates. 2. There was one unknown compound in the reaction that was later discovered after a series of techniques described above.
CML103 - Term paper Methanol Synthesis Industrial process/chemical synthesized: Today in industries, generally the basis for the manufacture of methanol is synthesis gas (normally called as syn gas). Syn gas is a mixture of carbon-monoxideand hydrogen. By syn gas :- For the production of methanol to be independent of feedstock material, the three steps that can be followed are :- Syn gas preparation, Methanol synthesis and, Methanol purification that contain the reactions given below a.) CO (g) + 2H2 (g) CH3OH (g)
The 250 mL beaker was rinsed well with the distilled water. The titration procedure above was repeated 2 more times with fresh potassium acid
Reaction is carried out in a 500 ml three-neck flask supported on a heating mantle and provided with a mechanical stirrer, a water condenser, a thermometer probe with an inlet for dry nitrogen gas, and an addition funnel. The calculated amount of IPDI and THF are charged to the three- neck flask under mechanical stirring and BTMSPA is added slowly from the addition funnel at a rate to maintain the reaction temperature below 50°c. After addition of BTMSPA is complete, mixture is stirred for additional 1 hour at room temperature. The completion of the reaction is verified by FT-IR following the disappearance of peak associated with NCO groups. The obtained solution is transferred to a single-neck flask and by using a rotary vacuum evaporator THF is distillate in two steps and replaced by dry ethanol to yield around 60-65% solution.