The collection and meta-analysis of reaction data were based on publications covering Minisci-type alkylation using carboxylic acids as radical precursors, as reviewed by Proctor and Duncton . Based on the consolidated data, a 24-well alkylation screening plate was designed using reaction conditions most frequently reported in the literature. The reaction variables included temperature, time, compound concentrations, and scale, optimized for minimal material consumption and ease of integration into the experimental workflow. The miniaturization of scale and the adaptation of concentration ranges described in the literature (c = 0.016 M, n = 0.8 µmol) resulted in solid conversion rates for literature test reactions at a frequently reported temperature of 80 °C for 18 hours. Since most of the reactions worked with ammonium persulfate ((NH 4 ) 2 S 2 O 8 ) as the oxidant, only a single oxidant was used on the plate. However, the observed variety in silver salts (catalyst) led to the inclusion of six different species (AgNO 3 , AgBF 4 , Ag-pTsOH, AgCF 3 SO 3 , AgCO 2 CH 3 , and AgSCF 3 ). With an additional four parameters available on the plate, on the basis of the literature data analysis, a variation of additives was chosen over different solvents. Consequently, TFA, H 2 SO 4 , HNO 3 , and a nonadditive control were selected to allow for a broad range of pKa values. As a solvent system, a mixture of MeCN and H 2 O with a 3:2 ratio was chosen (Figure ).