As mentioned earlier, this copper/TEMPO catalytic system prefers to oxidize primary hydroxyl group compared to secondary hydroxyl group. We observed that dimethyl sulfoxide (DMSO) solvent (used in the HTS experiment) gave superior primary alcohol (12a) oxidation chemoselectivity compared to acetonitrile (MeCN) solvent (used in the literature 39 ) (Fig. ). To investigate the observed solvent effects, Experiment Designer agent suggested that we could conduct oxidation kinetics study for different solvent. Recently, automated kinetic profiling has become an efficient tool to help researchers establish reaction kinetic models . However, similar to the HTS technology discussed above, it is still not a routine tool used in process development due to the high entry barrier for mastering automated hardware and intricate programming involved in fitting kinetics models. In order to avoid extensive coding and data analysis, Experiment Designer, Hardware Executor, Spectrum Analyzer, and Result Interpreter agents orchestrated to complete the kinetic study task, consisting of subtasks including kinetics experiment design, automated sampling experiments, proton nuclear magnetic resonance ( 1 H NMR) analysis, and kinetic model fitting and analysis (Fig. ). In kinetics experiment design, Experiment Designer planned a sampling schedule for time-course data collection. To provide an approximate reaction rate information for experimental design, we firstly monitored the reaction via TLC, and found that substrate 12a was rapidly consumed within the initial first hour reaction time and the reaction slowed down afterwards. Based on this observation, Experiment Designer proposed a sampling schedule spanning a 10-hour reaction period. Samples were to be collected at 10, 20, 30, 40, 50, 60, 120, 240, 360, 480, and 600 minutes, such that denser data points could be obtained during the early stage of the reaction when the reaction rate was large. Subsequently, Hardware Executor agent generated the OT-2 running code based on the experimental design proposed by the Experiment Designer. The coded OT-2 liquid handler procedure contained a series of operations for sampling, such as stopping the reaction's shaking, pipetting to sample, quenching the reaction in the sample, and resuming shaking. The compositions of the sampled reaction crude were analyzed by 1 H NMR. Instead of manual analysis of the NMR data, we provided Spectrum Analyzer agent with 1 H NMR spectra and approximate chemical shifts for characteristic hydrogen atoms in the substrate, product, and byproducts (overoxidation products). Spectrum Analyzer wrote a Python program according to the API documentation for the TopSpin NMR processing software to automate the analysis of NMR data, the procedure of which included identifying target peaks, performing peak integration, and calculating the compositions of the samples (Fig. ).