Microwave-Assisted Reflux in Organometallic Chemistry: Synthesis and Structural Determination of Molybdenum Carbonyl Complexes

摘要

The application of microwave heating to chemical syntheses, since first being reported in 1986(1), has grown rapidly such that now a wide range of organic and inorganic reactions have been conducted (2). Advantages include shorter reaction times, cleaner reaction products, and milder experimental conditions. Consequently there are a growing number of applications of microwave heating in the under-graduate laboratory curriculum (3). Most of these experiments use open beakers covered with a watch glass, a procedure of limited scope and of certain experimental hazards. Procedures using sealed Teflon or thick-walled Pyrex reaction vessels (2) are less controllable and are usually too dangerous for student laboratories. Of the hundreds of papers reporting the use of microwaves in chemical synthesis, only very few used the microwave-assisted reflux technique (4). We report the application of this technique in an undergraduate laboratory; its simplicity, safety, wide scope, and low cost make it very suitable for this purpose.