Pour out the cold water from the cold finger, open the side-arm tap and carefully remove the finger. Scrape the solid onto a filter paper and record the yield.The infrared and 1H n.m.r. spectra of the product are displayed on the wall near the experiment. The corresponding spectra of the organometallic sandwich compund ferrocene (-C5H5)2 are provided for comparison. You should attempt to assign the peaks in the n.m.r. spectra and to account for the general features of the IR spectra.
Next, place 0.75 g of Fe(-C5H5)(CO)2CH3 and 0.5 g of triphenyl phosphine in a 50 cm3 Schlenk tube D (Figure 2).Stopper and pass a very gentle stream of nitrogen over the mixture for about 10 min. (The outlet should be attached to a toluene bubbler.) Then reduce the flow to a minimum by partially closing the tap. Immerse the bottom 4 cm of the tube in an oil bath at 100-120°C for 1 hour.