High-throughput methods were employed to study the influence of reaction parameters on the synthesis of the metal-organic frameworks MOF-5 (Zn 4 O[(OOC) 2 ·C 6 H 4 ] 3 ) and HKUST-1 (Cu 3 [(OOC) 3 C 6 H 3 ] 2 (H 2 O) 3 ·xH 2 O). Thus, compositional parameters (metal salt, reagent concentrations, and pH) as well as process parameters (temperature, time) were investigated in order to establish reaction trends and fields of formation. A multiclave reaction block was used to perform the investigation of 24 different solvothermal reactions at a time. Attention was focused on the phase purity and the crystal morphology of the resulting compounds. The characterization of the samples was performed by X-ray powder diffraction and high resolution scanning electron microscopy. The experimental results show that the formation, phase purity, and morphology of MOF-5 and HKUST-1 are extremely sensitive to the synthesis parameters explored in this study.