We began our testing and validation of the platform with a Giese-type reaction via photocatalytic HAT activation of hydrocarbons. The reaction was conducted in the Signify Eagle flow photomicroreactor, utilizing tunable 0-144 W, 365 nm light LEDs. This choice allowed us to evaluate a robust and well-established chemistry in our laboratory (Figure ). Four optimization variables were selected for the reaction (Benzalmalononitrile concentration, THF loading, catalyst (TBADT) loading, and residence time). A total of nineteen experiments were conducted in a closed-loop fashion continuously for four hours. The initial phase involved six experiments, serving as a preliminary scan of the reaction space. Subsequently, the BO algorithm recommended one new experimental condition at a time, aiming to maximize the objective function (yield (%)). Within nine experiments, the platform achieved a yield of over 90% and began converging on the optimal conditions for the chemistry, resulting in a yield exceeding 95% for the desired product. Notably, the reaction demonstrated a detrimental effect of high light intensity, with the optimal range found to be between 20-50% of full power (28-72 W optical input power). These optimal conditions were then utilized for scaling up the transformation, confirming the AI-determined yield with an isolated yield of 99% (3.7 mmol scale).