The invention discloses a preparation method of 2-(inner-5-
norbornene-2, 3-dicarboximide)-1, 1, 3, 3-
tetramethylurea hexafluorophosphate, which comprises the following steps: 1, dissolving
tetramethylurea in a polar aprotic
organic solvent, and dropwise adding a chlorination
reagent to carry out chlorination reaction; 2, after the chlorination reaction is completed, cooling is conducted, then
hexafluorophosphate and N-hydroxy-5-
norbornene-2, 3-dicarboximide are sequentially added, then inorganic base is added in batches for a
condensation reaction, and the
molar ratio of N-hydroxy-5-
norbornene-2, 3-dicarboximide to
tetramethylurea is 1-1.5; and 3, filtering the reaction liquid, adding an
inert organic solvent into the filtrate, and recrystallizing, so as to obtain the finished product of the 2-(inner-5-norbornene-2, 3-dicarboximide)-1, 1, 3, 3-tetramethylurea
hexafluorophosphate, namely the 2-(inner-5-norbornene-2, 3-dicarboximide)-1, 1, 3, 3-tetramethylurea hexafluorophosphate. The method has the advantages of simplicity in operation, mild and controllable reaction, high product purity, high yield and suitability for industrial popularization.