Abstract A procedure for protiodesilylation of 1-(trimethylsilyl)-1-alkynes that involves the use of catalytic amounts of AgNO 3 and does not require the employment of KCN is described. This procedure allows for chemoselective deprotection of 1-(trimethylsilyl)-1-alkynes containing α-(trimethylsilyl) benzyl moieties, tert-butyldiphenylsilyl alkyl ethers or tert- butyldimethylsilyl aryl ether groups. However, it causes complete desilylation of 1-( ...