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This guide is based on the microwave(MW)-assisted synthesis of carbostyrils derivatives. It is divided into 4 chapters which include first an overview of transition-metal catalyzed carbon-carbon cross- and homocoupling reactions. Second, functionalized 4,4 -bisquinolones can be efficiently synthesized by MW-assisted palladium(0)-catalyzed cross-coupling reactions, or via nickel(0)-mediated homocouplings of 4-chloroquinolin-2(1H)-one precursors. Both methods are also applicable to other types of symmetrical biaryls. Third, a method for the gram-scale preparation of functionalized 4,4 -bisquinolones using a MW-assisted Ullmann-type homocoupling reaction is described. Fourth, the electronic spectra of biscarbostyrils, which exhibit unusual properties in comparison to the corresponding carbostyrils, were examined. Time-dependent density functional calculations of absorption and emission spectra of selected derivatives show good agreement with the corresponding experimental data.