We investigate a high throughput approach to polymer synthesis by employing photoinduced electron/energy transfer reversible addition-fragmentation chain transfer (PET-RAFT) polymerization. Polymerization of a broad range of monomers, including acrylates, methacrylates, acrylamides, and styrenic monomers, was achieved directly in a multiwell plate by employing 5,10,15,20-tetraphenylporphine zinc (ZnTPP) as a photocatalyst under yellow LED light. Various parameters such as monomer concentration and degree of polymerization were investigated with respect to their effect on polymerization rate and the degree of control over the molecular weight and molecular weight distribution. Finally, the synthesis of well-defined multiblock copolymers (up to a hexablock copolymer) was shown to be achievable entirely within a multiwell plate without any intermediate purification. The versatility and ease of this oxygen tolerant polymerization in high throughput formats make it an excellent technique for the generation of polymer arrays.