EXPT 4 PREPARATION AND CHARACTERISATION OF A FERROCENE DERIVATIVE Lab Manual Introduction Dicyclopentadienyliron or Ferrocene has the formula (-5-C5H5)2Fe. The Greek letter (eta) is used to indicate...

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write a lab report on the analysis of ferrocene derivative.make sure to include the calculations, result table and IR spectrum.the report should have the following:1. introduction2. lab method3. results/calculation4. discussion5.conclusion6. references


EXPT 4 PREPARATION AND CHARACTERISATION OF A FERROCENE DERIVATIVE Lab Manual Introduction Dicyclopentadienyliron or Ferrocene has the formula (-5-C5H5)2Fe. The Greek letter (eta) is used to indicate the number of carbon atoms that are bonded to the metal atom. When it was discovered that dicyclopentadienyliron underwent electrophilic substitution reactions e.g. Friedel-Crafts acylation, Vilsmeyer formulation etc., R.B. Woodward suggested the name “ferrocene” for the compound by analogy with benzene. In this experiment the acylation is carried out under mild conditions. The acylation system used, H3PO4/(CH3CO)2O produces a relatively small concentration of the active electrophile CH3C=O+. The product is separated from any side-products and unreacted starting material using TLC. It is characterised using IR. Experimental Add 0.2g of ferrocene to a 100 cm3 conical flask containing 1.2 cm3 of 85% H3PO4 and 8 cm3 of acetic anhydride. Protect the mixture from moisture with cotton wool plug in the neck of the flask. Heat the mixture on a steam bath for 3 minutes ± 20 sec. Remove from the steam bath and quickly pour the contents into a 250 cm3 beaker which is half filled with ice. Thoroughly mix the contents of the beaker using a glass rod. Carefully add NaHCO3 in small amounts with constant stirring until CO2 is no longer evolved i.e. no more “fizzing”. (The appearance of solid NaHCO3 remaining on the bottom of the beaker is a clear indication that this stage has been reached!). Cool the mixture on the ice bath for 15 min to precipitate the ferrocene from solution. Suction filter the solid and wash with water (50cm3) and allow to dry for 15 min. Obtain infra-red spectra of (a) pure ferrocene and (b) the product. Chromatography Using a 10 cm3 graduated pipette, prepare 10 cn3 of each of the following petroleum spirit:diethyl ether solvent compositions: 100:0; 90:10; 80:20; 70:30; and 50:50. Place these solvents in the dried developing tanks. Replace the lids. Prepare concentrated solutions in diethyl ether (ca. 1 cm3) using tiny amounts of (a) pure ferrocene and (b) your product in clean dry spot plates. Using capillary tubes, place a small spot of each of the two solutions on 5 separate TLC plates. Repeat if not intense enough. Ensure that the spots are above the level of the solvent in the developing tanks. Mark the position of the spots lightly with a pencil. When the plates are dry, place one in each of the developing tanks and replace the lids. Remove when the solvent has travelled approx. 80% of the plate. Mark the position of the solvent front. Calculate Rf values for both ferrocene and the product, where Rf = distance travelled by solute/distance travelled by solvent. Writeup 1. Examine the IR spectra and use with the chromatography results to elucidate the structure of the product. 2. Tabulate the Rf values and plot Rf against diethylether % for both ferrocene and the product. 3. Which of the solvent compositions would you use to separate gram quantities of the product from unreacted ferrocene using column chromatography? Reference 1. F.A. Cotton and G. Wilkinson in “Advance Inorganic Chemistry”, J. Wiley & Sons. RESULTS TABLE TO BE USED FOR LAB REPORT Yield Amount of ferrocene weighed out = 0.2004 g Amount of acetic anhydride weighed out = 8 ml Amount of ferrocene derivative produced after drying = 0.0985 g Determination of Rf values Petroleum ether: diethyl ether Solvent front Pure Ferrocene Product 100:0 49 mm 2 mm 53 mm 90:10 66.5 mm 17.5 mm 64 mm 80:20 79.5 mm 15.5 mm 77.5 mm 70:30 73 mm 23 mm 72 mm 50:50 51 mm 49.5 mm 62 mm IR SPECTRUM
Answered 3 days AfterApr 17, 2021

Answer To: EXPT 4 PREPARATION AND CHARACTERISATION OF A FERROCENE DERIVATIVE Lab Manual Introduction...

Shweta answered on Apr 20 2021
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Introduction:
We offer a list of good photo compounds and the oxidised forms in which simple neutron donation classes such as hydrogen or acetate groups on cyclopentadienyl-rings allow for fine tuning of Fe+III/Fe+II redox potentials from +0.403 V to 0.096 V versus a lithium met
al membrane. Time pairs of mannose and access to the quality compounds emulate human or monocyclic acyl Chuck schumer based binding affinities, resulting from either the evaporation of 2-aminobenzenthiol (L) with monoacetyl ferrocene in the molar ratio 1:1 or in the molar ratio 1:2 for formaldehyde ferocine have been prepared. HLa-Maf and H2Lb-Daf are the Schiff Base ligands that result from the polycondensation reaction. The sulphur in the thiol group, as well as the carbon atom in the imidazole ring of the ligands, chelate the binding sites to organic compounds. H2Lb-Daf is an often positively cargend schiff base binding site, whereas HLa-Maf is a benzoic sustainable economic growth or aliphatic enhance business performance binding sites. The connection of 1,1′-fc(SeLi)2, which is formed with 1,1′-fc(SeSiMe3)2 and n-BuLi, with authoritative of CpFe(CO)2I, yields new hetero compounds of the normal spinel 1,1′-fc[SeFeCp(CO)2]2 (fc = Fe(5-C5H4)2 (fc = Fe(5- At 50 °C and a 1:2 (metal/ligand) adsorbent dosage, photocatalytic Chairman processes of the organoiron diselenolate with bis-phosphines yielded 1,1′-fc(SeFeCp(PP)2. Chemical and physical and microscopy approaches were used to classify all of these groups. That addition of hydrogen and translate directly to the Cp-rings results in the classification and functional density theory (DFT) measurements of four distinct changed ferrocenes in the this article. His analysis offers an insight, however and in what degree the properties of ferrocene can be regulated or adjusted through the addition of a basic electrons donation device to the Cp-rings.
Lab Method:
In a 100 cm3 boiling tube 1.2 cm3 of 85 percent H3PO4 and 8 cm3 of acetic anhydride, add 0.2g of cyclohexanol. With a cling film plug in the flask's neck, shield the mix from humidity. Stir the solution for 3 minutes and 20 seconds in a steam bath. Drop the liquids from of the hot shower and dump them into a 250 cm3 flask partially of water. And use a capillary tube, stir the mixture the contents of the beaker. Continue adding NaHCO3 in small quantities, stirring constantly, until no CO2 is generated, i.e. no more "fizzing." (The presence of strong NaHCO3 on the side of the bottle is a sure sign that this level has also been achieved!). To catalyse the n - hexane from the water, chill the combination for 15 minutes in an ice bath. Vacuum clean the strong, then clean this with 50cm3 of water and let it dry for 15 minutes.
Infrared spectra of (a) pure ferrocene and (b) the substance...
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