2-(4-hydroxy-phenyl)-1,1,1,3,3,3-hexafluoro-propan-2-ol (1) was obtained from 2-(4-amino-phenyl)-1,1,1,3,3,3-hexafluoro-propan-2-ol (2) via diazotization and hydrolysis; The influence factors of diazotization and hydrolysis were investigated. The product was identified by EA, 1H NMR, IR and MS spectra. The results showed the optimum reaction conditions were as follows: during diazotization, w(H2SO4)=w(NaNO2)=30%, n(H2SO4) : n (NaNO2) : n (1) = 4.0 : 1.1 : 1.0, reaction temperature -2~2 ℃; during hydrolysis, w(H2SO4)=50%, n (H2SO4): n (1) = 11: 1.0, reaction temperature 108~112 ℃ and reaction time 2 h. Under these conditions, 91% 2-(4-hydroxy-phenyl)-1,1,1,3,3,3-hexafluoro-propan-2-ol was obtained.