In recent years, chemistry in flowing systems has become more prominent as a method of carrying out chemical transformations, ranging in scale from analytical-scale (microchemistry) through to kilogram-scale synthesis (macrochemistry). The advantages are readily apparentincreased control of conditions leading to greater reproducibility, scaleability, and increased safety/reduced lossalthough its acceptance as a viable synthesis technique has been limited due to its drawbacks, primarily precipitation, liquid handling, and diffusion of the reaction within the reactor. Here, we present details of a system which bridges the gap between micro- and macroreactors and has enabled fast reaction optimisation (using small amounts of reagents) and subsequent multigram scale-up using a commercial reactor.

No abstract

Microwave-assisted organic synthesis in a laboratory-scale monomodal microwave reactor is investigated for continuous flow applications using fluorous spacer technology. The benchtop continuous flow microwave described allows sequential processing of multiple plugs using small amounts of reagents for reaction optimization, scale-up and array synthesis. The system features online monitoring of temperature, pressure and microwave power. Several different reactions have been scaled up, including a Suzuki-Miyaura cross-coupling reaction and nucleophilic substitutions. In all cases it was possible to optimize the reaction conditions on a small scale (∼300 µL processing volume), and achieve similar conversions on an intermediate scale (∼30 mL), offering the potential for further scale-up without modifying the optimized conditions (direct scalability) producing similar isolated yields in the C-C bond formation reaction.

No abstract

No abstract