The explorations, observations, and lessons learned above culminated in a concise and scalable solution to the total synthesis of STX and related analogs as illustrated in Scheme 1C. Thus, requisite building blocks 30 and 32 were prepared on decagram scale from serine derivative 2 and proline (3). The former building block could be accessed via reduction and sulfinimine formation (using 39) to furnish 30 (67% yield over 2 steps) while the latter utilized the aforementioned biocatalytic C-H oxidation of 3 followed by one-pot alcohol protection/redox active ester (RAE) formation to afford RAE 32 in 40% overall yield from proline. The convergent radical coupling of 30 and 32 proceeded smoothly under reported conditions to deliver a single diastereomer of 33 on decagram-scale in 80% isolated yield.