A concise method to synthesize 2-styryl-3,5-diethoxycarbonyl-6-methylpyridine derivatives was established. The intermediate of 2,6-dimethyl-3,5-diethoxycarbonylpyridine was synthesized by cyclization of ethyl acetoacetate, formaldehyde and ammonium acetate and oxidative aromatization. Nine title compounds were synthesized by condensation of benzaldehyde derivatives and intermediate in the reflux of acetic acid. The structures of compounds were confirmed by 1HNMR, MS and IR. The fluorescence spectral characteristics in different solvents of pyridine derivatives were studied, the results show that the maximum absorption wavelengths of pyridine derivatives in different solvents were between 302~382nm, emission wavelengths were between 397~537nm, molar extinction coefficients in 1.045×10-4 ~ 4.236×10-4L•mol-1•cm-1.