A New Microwave Reactor for Batchwise Organic Synthesis

Article abstract of DOI:10.1021/jo00113a028

A laboratory-scale microwave batch reactor (MBR) has been developed for organic synthesis or kinetic studies on the 20-100 mL scale, with upper operating limits of 260 deg C and 10 MPa (100 atm).The MBR complements a continuous microwave reactor which was the subject of a previous report from the author's laboratory.Microwave-assisted organic reactions were conducted safely and conveniently in the MBR, for lengthy periods when required, and in volatile organic solvents.The use of water as a solvent for organic reactions was also explored.Examples include oxidation, elimination, esterifications, hydrolysis of a tertiary amide, etherification, isomerization, Hofmann elimination, α-iodination of a carboxylic acid, Claisen rearrangement, aminoreductone formation, and Willgerodt reactions.Advantages of the new MBR include the capability for rapid heating and quenching of reaction mixtures, minimal temperature gradients within the sample, and elimination of wall effects.Safety aspects have been discussed.