While synthetic organic chemists have taken advantage of microwave heating in their work, there have been relatively few reports of application in preparative organometallic chemistry. Microwave heating offers several advantages over conventional methods include significant rate acceleration and, in many cases, improved product yields and selectivity. A major problem with performing organometallic chemistry using microwave heating is that, in ligand exchange reactions, stopping a reaction after a desired number of substitutions is difficult if the reaction cannot be continually monitored. With in-situ Raman apparatus we can monitor reactions in real time and can carefully control the synthesis of organometallic compounds. In addition, by using gas-loading equipment we can perform reactions under an atmosphere of reactive gases. This has allowed us to prepare a number of key organometallic compounds very quickly and efficiently. Our results will be presented here.