A protocol for conducting Suzuki reactions in a plate format amenable to use in library synthesis of biaryl compounds has been developed. A key objective was to determine reaction conditions which give biaryl products containing <10 ppm of Pd for a wide variety of building blocks. A Design of Experiments (DoE) approach for the identification of an optimised set of reaction conditions was successfully applied. The utility of the protocol developed has been demonstrated by preparation of an array of 96 biaryl compounds in a parallel fashion.