Diverse alkali metal thioselenophosphinates, M[SeSPR 2 ] (M = Li, Na, K, Rb, and Cs; R = alkyl, aryl, aralkyl, and hetaralkyl), have been synthesized in 78-94 % yields by means of a one-pot multicomponent reaction between secondary phosphanes, sulfur, selenium, and alkali metal hydroxides under mild conditions (room temperature, -50°C, 0.5 h, EtOH). The molecular and electronic structure of the [SeSPPh 2 ]anion and its coordination behavior towards Li + , Na + , and K + cations have been investigated at the B3LYP level of theory. The alkylation of the alkali metal thioselenophosphinates with various organic halides proceeds regiosecifically at the selenium center to form Se-organyl thioselenophosphinates, Siberian Branch of the Russian Academy of Sciences, 1 Favorsky Str., 664033 Irkutsk, Russian Federation

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The reaction of tri(2‐pyridyl)phosphine with electron‐deficient alkynes in water proceeds under mild conditions (40–45 °C, without catalyst, 4–5 h) with liberation of pyridine to give (E)‐pyridylvinylphosphine oxides in 45–56 % yields, the only exception being the reaction with cyanophenylacetylene, which affords the corresponding vinylphosphine oxide of Z‐configuration in 40 % yield. The reaction is likely triggered by the zwitterion, the adduct of tri(2‐pyridyl)phosphine to the electrophilic acetylenes, the carbanionic center of which is then neutralized by a proton from water. The intermediate phosphonium hydroxide finally decomposes to the product.