Under mechanochemically induced conditions, a wide range of diarylphosphine oxides or -phosphonates react with trisulfide dioxides to afford various thiophosphate derivatives in good yields. Selective S-S bond cleavage of trisulfide dioxides determined by connecting groups is proposed as the key step in the construction of P(O)-S or P(O)-S-S bonds, which is supported by calculations.
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