The invention discloses a preparation method of 2, 3, 5, 6-phenylcarbinol 
tetrafluoride; the preparation method is as follows: the 2, 3, 4, 5, 6-cyanobenzene 
pentafluoride is taken as initial 
raw material; cyano group is firstly reduced by 
catalytic hydrogenation, and then diazotization and 
hydrolysis reaction are carried out for obtaining 
hydroxide radical, and then contraposition defluorination is carried out for obtaining the 2, 3, 5, 6-phenylcarbinol 
tetrafluoride; or the 2, 3, 4, 5, 6-cyanobenzene 
pentafluoride is taken as initial 
raw material, the contraposition defluorination is carried out for obtaining the 2, 3, 5, 6-cyanobenzene 
pentafluoride, the 
hydroxide radical is reduced by the 
catalytic hydrogenation, and then the diazotization and the 
hydrolysis reaction are carried out for obtaining the 2, 3, 5, 6-phenylcarbinol 
tetrafluoride. The two synthetic routes of the invention both comprises the three reaction steps of 
catalytic hydrogenation, diazotization and 
hydrolysis and contraposition defluorination; wherein, in the catalytic 
hydrogenation process, acid is added for obtaining amine salt, and the diazotization and the hydrolysis reaction are carried out by a one pot process, thus leading byproducts to be greatly reduced, the main products to have high purity and the yield coefficient to reach more than 74 percent; in addition, the whole process has simple operation, mild reaction condition and cheap and easily obtained 
raw material; catalyst and 
solvent can be recycled and used, thus reducing 
pollution, being environment-friendly, having economic value and being suitable for industrialization.