Allowing many chemical reactions to be completed within minutes, microwave heating has revolutionized preparative chemistry. As a result, this technology has been widely adopted in both academic and industrial laboratories. Integrating microwave-assisted chemistry into undergraduate laboratory courses enables students to perform a broader range of reactions in the allotted lab period. As a result, they can be introduced to chemistry that would otherwise have been inaccessible due to time constraints (for example, the need for an overnight reflux).
Laboratory Experiments Using Microwave Heating provides 22 experiments encompassing organic, inorganic, and analytical chemistry performed using microwave heating as a tool, making them fast and easy to accomplish in a laboratory period. Utilizing the time-saving experiments described in this book also permits students to repeat experiments if necessary or attempt additional self-designed experiments during the lab course.
A number of the chemical transformations use water as a solvent in lieu of classical organic solvents. This contributes to greener, more sustainable teaching strategies for faculty and students, while maintaining high reaction yields. All the experiments have been tested and verified in laboratory classes, and many were even developed by students. Each chapter includes an introduction to the experiment and two protocols—one for use with a smaller monomode microwave unit employing a single reaction vessel and one for use with a larger multimode microwave unit employing a carousel of reaction vessels.
Table of Contents
Introduction: Using Microwave Heating in Chemistry: The Basics
Experiment 1 Diels–Alder Cycloaddition Reaction
Experiment 2 Second-Order Elimination Reaction: Preparation of Heptene from 2-Bromoheptane
Experiment 3 An Addition–Elimination Sequence: Preparation of a Bromoalkene
Experiment 4 Fischer Esterification: Preparation of Ethyl-4-Aminobenzoate (Benzocaine)
Experiment 5 Transesterification Reaction: Preparation of Biodiesel
Experiment 6 Knoevenagel Condensation Reaction: Preparation of 3-Acetylcoumarin
Experiment 7 The Perkin Reaction: Condensation of an Aromatic Aldehyde with Rhodanine
Experiment 8 Williamson Ether Synthesis: Preparation of Allyl Phenyl Ether
Experiment 9 Claisen Rearrangement: Preparation of 2-Allyl Phenol from Allyl Phenyl Ether
Experiment 10 Hydration of an Alkyne: Preparation of Acetophenone from Phenylacetylene
Experiment 11 Oxidation of a Secondary Alcohol: Preparation of a Ketone
Experiment 12 Suzuki Coupling Reaction: Preparation of a Biaryl
Experiment 13 Heck Reaction: Preparation of Substituted Cinnamic Acids
Experiment 14 Preparation of an Aryl Nitrile: Application of a Copper-Catalyzed Cyanation Reaction
Experiment 15 Alkene Metathesis: Preparation of a Substituted Cyclopentene
Experiment 16 Click Reaction: Preparation of a Triazole
Experiment 17 Coordination Chemistry: Preparation of Cisplatin
Experiment 18 Preparation of a Palladium Complex: Bis(triphenylphosphine)Palladium(II) Dichloride
Experiment 19 Coordination of an Aromatic Ring to a Metal: Preparation of an Arene Chromium Tricarbonyl Complex
Experiment 20 Determination of an Empirical Formula: Zinc Bromide
Experiment 21 Microwave-Assisted Extraction: Identification of the Major Flavor Components of Citrus Oil
Experiment 22 Microwave-Assisted Digestion of Dietary Supplements: Metal Analysis by Atomic Absorption Spectroscopy
Nicholas E. Leadbeater, PhD, is an associate professor of chemistry at the University of Connecticut. Dr. Leadbeater’s research interests are focused around development of new synthetic methodology, with an emphasis on cleaner, greener routes to known and novel compounds. Dr. Leadbeater has a passion for undergraduate education, both developing new lecture and laboratory classes and incorporating undergraduate students into research. He was the recipient of the 2010 University of Connecticut College of Liberal Arts and Sciences Excellence in Teaching Award in the Physical Sciences.
Cynthia B. McGowan, PhD, is a full professor of chemistry at Merrimack College, North Andover, Massachusetts. Her pioneering work in the use of microwave technology for organic chemistry experiments and teaching is "student-tested" and refined. A committed and popular undergraduate teacher, recognized by her peers with a teaching excellence award in 1999, she continues to adapt her material to the ever-changing world of technology so that her students are well prepared for graduate work or positions in industry.
"The book starts with a short and easy-to-understand introduction to the basics of microwave heating, which in my opinion every microwave user should know. … Designed as a textbook for the undergraduate laboratory, Laboratory Experiments Using Microwave Heating is a valuable addition to the range of microwave books available. It is the first to include inorganic and analytical chemistry experiments, and will help students to become acquainted with microwave technology at an early stage."
—Chemistry World, 2014