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A novel efficient method for the synthesis of thiophosphate derivatives catalyzed by methylene blue with blue light irradiation under an air atmosphere is described. The thiophosphate products, which are found in many pharmaceuticals and pesticides, were obtained in moderate to good yields. Moreover, Stern–Volmer fluorescence quenching experiments were conducted on reaction partners, demonstrating that the transformation involves photoinduced electron transfer. A plausible mechanism is proposed.