In this work, a new reaction-based red to near-infrared (NIR) fluorescent turn-on probe for H2S was developed. This probe uses a readily prepared dicyanoisophorone as the fluorophore and a 2, 4-dinitrobenzenether with an ortho-aldehyde group as the reaction site. Upon addition of H2S, a fast nucleophilic addition of H2S to the aldehyde group and a following efficient intramolecular thiolysis of dinitrophenyl ether occurred, which leads to release the fluorophore and give a rapid NIR fluorescence turn-on response for H2S with a super large Stoke...