Herein we develop a T3P-promoted synthetic methodology to construct phosphonodithiolates in acetonitrile (See supporting information for details) (Figure ). We further test if this reaction be performed in aqueous solution. we found that both phosphonodithiolate and phosphonothiolate formed when the reaction was moved in aqueous solution (Figure2 &3a). However, the phsophodithiolate can further hydrolyze to phosphonothiolate with time (Figure2 &3a). This reaction cascade formed at the cost of consuming T3P as the chemical fuel. Notebly, we found that transient droplets form with the generation of phosphonodithiolate (Figure ). The concentration of PO(n-Pr)(p-OMePhS)₂ then underwent decay over time. After 3.5 hours, PO(n-Pr)(p-OMePhS)₂ was almost completely consumed, while PO(n-Pr)(p-OMePhS)(OH) reached the highest concentration. We continued to monitor the concentration variation of PO(n-Pr)(p-OMePhS)(OH) for up to 23 hours and observed no further hydrolysis, with its concentration remaining stable over time.