A very mild method for the introduction of functionalized alkylselenyl group at C‐3 position of the indole ring was developed. The proposed procedure consists of an electrophilic substitution of indole and its derivatives with bis(O,O‐diisopropoxyphosphorothioyl) diselenide and subsequent cleavage of the P–Se bond with tetrabutylammonium fluoride in the presence of various electrophilic reagents. This method can be successfully applied, inter alia, for the preparation of amino acid and glucoside derivatives of 3‐selenoindole.
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