The invention discloses a method for preparing 5-fluorosalicylaldehyde from p-fluorophenol, and belongs to the technical field of
organic synthesis. A mild
formylation method is realized by innovatively adopting a catalyst and an active
methylene derivative (POCl3 + DMF) as a C1 source. According to the method, p-fluorophenol is taken as a
raw material, in the presence of a catalytic amount of
titanium tetrachloride, p-fluorophenol,
phosphorus oxychloride and N, N-
dimethylformamide are subjected to Vilsmeier-Haack reaction in
dichloromethane to synthesize p-fluorobenzaldehyde, and then a
methanol-water recrystallization process is adopted to replace
distillation for purification. Core improvements include: (1)
titanium tetrachloride catalyzes Vilsmeier-Haack reaction, and by-products are few; (2) the temperature is controlled by stages, and the operation is easy to control; (3) directly dropwise adding reaction liquid to hydrolyze at 10-25 DEG C; and (4)
methanol / water recrystallization purification. According to the method, the defects of a traditional process are overcome, the purity of a crude product reaches 85%-92%, the purity after recrystallization is larger than or equal to 98.5%, the yield is stabilized at 88%-91%, and the method is easy and convenient to operate, low in
energy consumption,
environmentally friendly and easy to industrialize.