wv EXPERIMENT 4 PREPARATION OF FERROCENE (II-C.H).Fe Cho "Ferrocene be discovered (abou rember ofthe socalled “sandwich” compounds to the following structure: tech of the 10 carbon atoms. The rings are nearly eclipsed in aso in the related Ruthenium and Osmium. complexes. Here the second produc is only obtained in small ids since subsequent acetylation Is deactivated. ‘Atematively, the acetyletion of ferrocene can be carried out under milder conditions to yield primaniy the monoacetyl product, using acetic anhydride in phosphvic acd Chloride with AICI ony the monoacety| is produced in this case. In this experiment, you wil prepare ferooene and compare the nm. spectrum of ‘the pure material to that found forthe product from the reaction with acety chloride. PREPARATION Gethylamine method summarised by the equations2FoCl, + Fo —>3FeCl, FeCh + 2H, + 2EuNH —> + 2ENHHCI However the method you wi employ uses an approach suggested only recenty ‘Alkali metal hydroxides which are ininsically very strong base may be used in a ‘nonchydroxviic sor eproronate an 1A. This Ie easily accom: ‘excess because (0 form a stable viz. 2KOH(s) + HA» Kee + A: + KOHH,O'S) “The reactions involved inthe synthesis ae 2KOH + C, Into the second boiling tube place 10 ml of dimethyl sulphoxide and 2 9 of anhydrous ferous chloride jon and the tubes sheken,[Ater standing for 30 minutes filer off the exystaline product and dry at ‘This last fitration may be carted out percentage based on FeCl, and the m.pt. pump. the laboratory. Record your yield asa lerature value should be compared) WRITE-UP QUESTIONS ) Whi the significance of the prof 1Tin the formula of ferrocene? ) Why Is ferrocene the most M(CiH). where M isa first row fof the compounds of the general formula sition element? (9 The *H' nm. spectra for ferrocene and the produet from reaction with acetyl chloride are given in the appendix. Record the chemical shifts and account for the differences of the H's in the acetylated ring of Fe(CyHs) (CyH{COMe) as ‘compared to that of the H's in the monoacetylated rng. ) What isthe use of DMSO and KOM in this synthesis? ) ctrophilc substitution reaction ‘ing of (Cp)sFe faster than that ofthe Friedal Craft reaction on benzan: REFERENCES ) Cotten and Wilkinson. Advanced inorganic Chemistry sis and Technique in Inorganic Chemistry*anges wun a ing Ta 2) Student ae age of at a rs oo eas vee