The invention discloses coumarin-oxacalix[3]arene fluorescent reagents as well as a preparation method and application thereof, and belongs to the fields of organic synthesis and analytical chemistry. The invention respectively synthesizes two coumarin-oxacalix[3]arene fluorescent reagents: chemical name a: 7,15,23-tertiary butyl-25,26,27-tri{1-[N-(7-coumarin oxyethyl)-1,2,3-triazole]-4-methoxy}-3,11,19-trioxacalix[3]arene; b: 7,15,23-triethoxycarbonyl -25,26,27-tri{1-[N-(7-coumarin oxyethyl)-1,2,3-triazole]-4-methoxy}-3,11,19-trioxacalix[3]arene. Meanwhile, the invention discloses a synthesis method and process conditions. According to the invention, the two coumarin-oxacalix[3]arene fluorescent reagents, in detecting ferric ions, have characteristics of high selectivity and high sensitivity; the fluorescent reagents are applicable to qualitative and quantitative analysis.