The purpose of this experiment was to identify the unknown alkyl bromide and ketone using a Grignard reaction and IR spectrum. Also, retrosynthesis analysis was used to determine the success of identifying starting material. The organometallic compounds have a carbon-metal bond that is used to create alcohol and to expand chains of carbons. Grignard reagents, a part of organometallic ionic compounds, are widely used in organic synthesis because they are considered strong base, strong base carbon nucleophile, and soluble in many organic solvents. Results: Alkyl bromide #24 and alkyl ketone #24 was assigned. During the first week of the experiment, the Grignard reagent was prepared from an alkyl bromide and magnesium. During the hydrolysis, …show more content…
At 3411 cm-1, it had a broad peak which means that it contained the alcohol, -OH. Carbonyl group was reduced to an alcohol. There was also C-H stretch at 2958.29 cm-1 and 2873.29 cm-1. There was a peak at 1716.94 cm-1 which means that C=O ketone bond exists in the final product. A C=O ketone bond is found in the 2-butanone, the starting ketone sample in this experiment. The presence of that peak indicates that some ketones were carried with the …show more content…
The presence of ketone in IR shows that all of the ketones did not react to form the Grignard reagent because the magnesium oxidized or there was still water remains in the funeral which makes the Grignard reagent to react with water instead. Once the magnesium is oxidized, it would not react again. Therefore, it is necessary to make sure the apparatus dry enough before the experiment. When thermocouple was placed into the glassware, the measuring tip was not in the neck of the distillation head and far away from the insulated. As a result, the resultant boiling point of alcohol would be lower than the actual boiling point. In the future experiment, making sure the thermocouple is in the right position is important to obtain an actual boiling point of its compound. Also, when reaction flask was placed in the ice bath, the solution was left in the cool longer than supposed to be. The rate of the reaction increases with the temperature, so cooling the reaction too much will stop the reaction. The Grignard reagent could not form if the reaction stops. It is important to cool the reaction moderately and stop when the vapors do not come out of the
Magnesium is added to a capped and dried flask with a crystal of iodine, ether and a drop of 1,2-dibromoethane. The iodine was essential to activate the magnesium. Ether was used as the solvent because there are no acidic hydrogen’s on ether that can potentially react with the Grignard reagent and also because ether has two lone pairs on the oxygen that can help to stabilize the magnesium
The goal of the experiment is to synthesize a bromohexane compound from 1-hexene and HBr(aq) under reflux conditions and use the silver nitrate and sodium iodide tests to determine if the product is a primary or secondary hydrocarbon. The heterogeneous reaction mixture contains 1-hexene, 48% HBr(aq), and tetrabutylammonium bromide and was heated to under reflux conditions. Heating under reflux means that the reaction mixture is heated at its boiling point so that the reaction can proceed at a faster rate. The attached reflux condenser allows volatile substances to return to the reaction flask so that no material is lost. Since alkenes are immiscible with concentrated HBr, tetrabutylammonium bromide is used as a phase-transfer catalyst.
Specific to the experiment, the distillation technique will be used to separate the two miscible liquids, conclude their identities based on the boiling points
There are numerous ways for the synthesis of organic esters and most of which have been briefly studied by Yadav and Mehta 7. The simple and old route for preparing esters is by the reaction
The evaporating dish was placed on top of the wire gauze and covered with the watch glass. The Bunsen burner was used to heat the water to a boil until the water had evaporated, leaving a dry, white solid (salt). The evaporating dish with the watch glass containing the salt residue was then weighed and recorded to 0.001 g. The mass of the evaporating dish and watch glass containing the salt residue was subtracted from the mass of just the evaporating dish and watch glass which gave the mass of the
6 H2O) in 100 ml distilled water. (vi) 0.2(N) Sodium Hydroxide solution: Dissolve 8.0 gm sodium hydroxide in 1 l distilled water. (vii) Acetic acid: Dilute 1 part of glacial acid with 4 parts of water. (viii) Stock cyanide solution: Dissolve 2.51 gm potassium cyanide (A.R. Grade) in 1 l water, standardize this solution with 0.0192(N) silver nitrate solution.
The beaker was placed on the heating element on high heat and was left undisturbed until it began to boil. When the solution reached a rolling boil, the temperature of the water was tested and recorded utilising the same method as the first trial. Two more trials of the 0.5 M mixture were conducted. The experiment was repeated three times more with 11.688 grams of salt to create a 1 M mixture. The experiment was repeated three times more with 17.532 grams of salt to create a 1.5 M mixture.
The purpose of this experiment is to perform a two step reductive amination using o-vanillin with p-toluidine to synthesize an imine derivative. In this experiment, 0.386 g of o-vanillin and 0.276 g of p-toluidine were mixed into an Erlenmeyer flask. The o-vanillin turned from a green powder to orange layer as it mixed with p-toludine, which was originally a white solid. Ethanol was added as a solvent for this reaction. Sodium borohydride was added in slow portion as the reducing agent, dissolving the precipitate into a yellowish lime solution.
Referring to the table of derivatives, which one aldehyde or ketone is most likely her unknown? Explain your reasoning, if she is unsure what conclusion to draw, what experiment should she do next? • Judging by those two melting points, acetophenone is most likely her unknown. The listed melting point for Oxime is 60°C and the listed melting point for Semicarbazone is 203°C. The melting points she derived are marginally lower, which is an indicated of slight impurity.
Nevertheless, the latter is not used in this experiment since it is very reactive and extremely flammable. On the contrary, NaBH4 is relatively mild and it can be used with protic solvents. In this manner, 1.507 grs of the ketone 9-fluorenone were mixed with 30.0 ml of 95% ethanol in a 125 ml Erlenmeyer flask. The bright yellow mixture was stirred during 7 minutes until all the components were dissolved.
Kolbe-Schmitt Reaction Kira Wall (CHE433) 12-3-14 The Kolbe-Schmitt reaction is named after Hermann Kolbe and Rudolf Schmitt. Schmitt published his research in the Journal fur Pracktische Chemie in 1885 while Kolbe published his research in the Annalen der Chemie und Pharmacie in 1860. The reaction adds a carboxyl group onto the benzene ring of a phenol.
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.
They are then passed from molecule to molecule until they reach an electron acceptor at the reaction centre where NADPH and ATP are produced, they are consumed by a light-dependant process that uses CO2 to form carbohydrates. Phillipe Barbier, a french chemist in the nineteenth century, discovered a way to produce a small amount of dimethyl heptanol by reacting methyl iodide, magnesium and methyl heptanone together under anhydrous conditions. Following his discovery, his student, Victor Grignard found out that by performing a reaction in different steps will produce a higher yield. The Grignard Reagent which can be reacted with a range of carbonyl-containing compounds to form an alcohol can be produced by reacting alkyl halide and magnesium using dry ether as a
The unknowns were correctly identified due to the clear presence of two plateaus in the experimental data. The hot plate was not turned on too high or too low to not obtain one of the three samples, and a sufficient number of values were taken in each part of the distillation before the mixture evaporated away to obtain approximately accurate data for boiling points. The ratio calculated for the volume of solvents in the mixture was .506/.488, where the composition of the mixture was 50.6% acetone, and 48.8% toluene. These two values did not add up to 100% because the GC also recorded some impurities,
Introduction Grignard reagent is considered as an organometallic compound or it's the composition of electrophilic and nucleophilic that electrophilic is the carbon atom of organic halide which is directly attached to the halogen, it's reactivity can be switched to the nucleophilic reactivity by conversion an organomagnesium halide. It has the general formula of (RMgX) and it has a general nomenclature which it's called magnesium alkyl halide. We can get Grignard reagent by adding one of solutions of alkyl halide to an ether, slowly. Then, garbling them that's leads to the boiling of solution and magnesium becomes disappeared so, we can get the reagent. Grignard reagent is also considered as the best known reagent of all organometallic compounds, as carbon atom is connected to a metal atom which may be