CER Labs 2-3 Figure 1. Friedel-Crafts Acylation. Claim: An acetyl group was efficiently introduced to ferrocene by Friedel-Crafts Acylation (Figure 1). We isolated our crude yield while comparing 2 purification techniques: column chromatography and recrystallization. TLC, NMR, and IR spectroscopy were used throughout the process to identify ferrocene and acetylferrocene in addition to evaluating the levels of purity.
Task 1 M1 Describe the scientific principles behind each of the three procedure above. Vacuum filtration is a procedure when a sold needs separating from a solvent to react the mixture. Then the mixture of a solid is measured through the filtration paper in a Buhner funnel. The liquid is drained through the funnel into the flask. Equipment • Filter paper • Buhner funnel • Tubing • Clean solvent • Disposable dropper Method 1.
The main objective of this experiment was the formation of phenacetin from the synthesis of acetaminophen. This was done through a chemical reaction known as the Williamson ether synthesis using techniques of refluxing, vacuum filtration and recrystallization incorporating a mixed solvent system. A further objective of this experiment was to study the formation of the product (phenacetin). Such validation was completed by using techniques for determining the melting point, calculating percent yield, and IR (infrared spectroscopy) of the resultant product. Our reaction yielded 3.696% of phenacetin product.
The reaction that occurs can be investigated via the adding of the liver extract which contains the arginase to urea concentrations and distilled water. The amount of urea formed is determined via spectrophotometric analysis α-INPP. The urea produced was known via the color reaction with the α-INPP, it is the reagent used for the colorimetric determination of urea. (Barry J, et al. 1984).
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.
Used solvents contain contaminants that can be removed by fractional distillation. The recycled solvents have purities suitable for re-use. Fractional distillation is used to separate the crude oil into its various components such as gasoline, kerosene oil, diesel oil, paraffin wax, liberating oil. Fractional distillation is also used for the purification of water. Water contains many dissolved impurities; these can be removed by this process.
Sample injection system This allows introduction of the analyte mixture into the stream of the mobile phase before it enters the column. Sample injector is made by means of a syringe and self-sealing septum of silicone, neoprene, or Teflon. Modern injectors are auto samplers, which allow programmed injections of different volumes of samples that are withdrawn from the vials in the auto sampler tray. 5. Column It is heart of HPLC system made up of heavy-walled glass tubing or precision-bore stainless steel.
Water acts as a leaving group in the third step and is removed from the reaction intermediate. In the fourth step, the molecule undergoes deprotonation with the help of the concentrated sulfuric acid to form isopentyl acetate. The reaction that was carried out in the experiment was a reversible reaction. In order to obtain as much isopentyl acetate as possible, Le Chatelier’s principle was used to ensure that we were able to collect a sufficient amount of isopentyl acetate. Le Chatelier’s principle says that if you disturb a system in equilibrium the equilibrium will shift in order to account for the disturbance.
Because it is a tertiary benzylic halide, the reaction is considered an SN1 type. To test the purity, the class then uses a TLC. When one places,” a spot of the substance on the absorbent surface of the TLC plate, the solvent (or solvents) run up through the absorbent,” (Zubrick223). The initial mass of the reactant, triphenylmethyl chloride was 2.006 grams. The experiment yield is 1.589g, which is a 80.3% yield.