A parallel synthetic approach toward homogeneous atom‐transfer radical polymerization of methyl methacrylate has been successfully applied by utilizing an automated synthesizer. Experimental set‐up, automated parallel synthesis and purification of the polymers via a solid‐phase extraction set‐up, as well as online and offline measurements of the molecular weights and monomer conversion are described in detail. In addition, a comparison with conventional experiments in the laboratory is provided.
Kinetic plots of ln(M]0/M]) versus reaction time of the ATRP of MMA in p‐xylene at 90 °C conducted in an automated synthesizer (three parallel reactions, ○, ▵, ⋄) and in a conventional set‐up (▪).
