Design and Performance Validation of a Conductively Heated Sealed-Vessel Reactor for Organic Synthesis.

A newly designed robust and safe laboratory scale reactor for syntheses under sealed-vessel conditions at 250 °C maximum temperature and 20 bar maximum pressure is presented. The reactor employs conductive heating of a sealed glass vessel via a stainless steel heating jacket and implements both online temperature and pressure monitoring in addition to magnetic stirring. Reactions are performed in 10 mL borosilicate vials that are sealed with a silicone cap and Teflon septum and allow syntheses to be performed on a 2-6 mL scale.

Design and evaluation of improved magnetic stir bars for single-mode microwave reactors.

Magnetic stirring in sealed cylindrical vessels designed for use in single-mode microwave instruments is typically less than optimal, and is not comparable to the efficient agitation that can be generally obtained in a round-bottomed flask fitted with a suitable magnetic stir bar or using overhead mechanical stirring systems. A new "vertical blade" stir bar design that improves the stirring performance in the very narrow, flow-constricting microwave vessels has been developed and evaluated for several different transformations where stirring and efficient agitation are known to be of importance. The better performance of these novel stirrers compared to the traditional cylindrical stir bar design is not only due to the geometry of the stirrer but also to the utilization of a magnetic material with a stronger magnetic transmission force (Sm2Co17) compared to standard ferrite or AlNiCo alloys.

Microwave-assisted and continuous flow multistep synthesis of 4-(pyrazol-1-yl)carboxanilides.

A series of 4-(pyrazol-1-yl)carboxanilides active as inhibitors of canonical transient receptor potential channels were synthesized in an efficient three-step protocol using controlled microwave heating. The general synthetic strategy involves condensation of 4-nitrophenylhydrazine with appropriate 1,3-dicarbonyl building blocks, followed by reduction of the nitro group to the amine, which is then amidated with carboxylic acids. Compared to the conventional protocol a dramatic reduction in overall processing time from ~2 days to a few minutes was achieved, accompanied by significantly improved product yields.

Sintered silicon carbide: a new ceramic vessel material for microwave chemistry in single-mode reactors.

Silicon carbide (SiC) is a strongly microwave absorbing chemically inert ceramic material that can be utilized at extremely high temperatures due to its high melting point and very low thermal expansion coefficient. Microwave irradiation induces a flow of electrons in the semiconducting ceramic that heats the material very efficiently through resistance heating mechanisms. The use of SiC carbide reaction vessels in combination with a single-mode microwave reactor provides an almost complete shielding of the contents inside from the electromagnetic field.

Electromagnetic simulations of microwave heating experiments using reaction vessels made out of silicon carbide.

There is a growing body of literature which reports the use of silicon carbide vessels to shield reaction mixtures during microwave heating. In this paper we use electromagnetic simulations and microwave experiments to show that silicon carbide vessels do not exclude the electric field, and that dielectric heating of reaction mixtures will take place in addition to heat transfer from the silicon carbide. The contribution of dielectric heating and heat transfer depends on the dielectric properties of the mixture, and the temperature at which the reaction is carried out.

Understanding microwave heating effects in single mode type cavities-theory and experiment.

This paper explains the phenomena which occur in commercially available laboratory microwave equipment, and highlights several situations where experimental observations are often misinterpreted as a 'microwave effect'. Electromagnetic simulations and heating experiments were used to show the quantitative effects of solvent type, solvent volume, vessel material, vessel internals and stirring rate on the distribution of the electric field, the power density and the rate of heating. The simulations and experiments show how significant temperature gradients can exist within the heated materials, and that very different results can be obtained depending on the method used to measure temperature.

On the importance of simultaneous infrared/fiber-optic temperature monitoring in the microwave-assisted synthesis of ionic liquids.

The temperature profiles obtained from both an external infrared and internal fiber-optic sensor were compared for heating and synthesizing the ionic liquid 1-butyl-3-methylimidazolium bromide (bmimBr) under microwave conditions. Utilizing a single-mode microwave reactor that allows simultaneous infrared/fiber-optic temperature measurements, significant differences between the two methods of temperature monitoring were revealed. Due to the strong microwave absorptivity of ionic liquids and the delay experienced in monitoring temperature on the outer surface of a heavy-walled glass vial, external infrared temperature sensors can not be used to accurately control the temperature in the heating of ionic liquids under microwave conditions.