This invention discloses a continuous method for preparing 3-difluoromethyl-1-methyl-1H-
pyrazole-4-
carboxylic acid based on a cascaded process of cyclization-de-alcoholization-scraped membrane fluorination, belonging to the field of continuous synthesis technology in fine chemicals. The method includes: cyclizing ethyl 2-ethoxymethylene-4,4-dichloroacetoacetate with
methylhydrazine in a loop reactor with forced external circulation, controlling the circulation ratio boundary at 15:1 to 18:1 to improve the selectivity of the target isomer; continuously removing at least some
ethanol from the cyclized liquid and adding
sulfolane for
solvent replacement, ensuring that the
ethanol content in the
system before entering the fluorination stage is no higher than 1.0% (wt) and the
water content is 0.1-0.2% (wt); subsequently, the resulting intermediate material, along with
anhydrous potassium fluoride and 18-crown-6 to form a heterogeneous
slurry, is fed into a vertical scraped
membrane reactor, with a
residence time strictly controlled at 169-171°C for 80-100 seconds, and rapid cooling within 3 seconds
after discharge; finally, the target product is obtained through
hydrolysis and acidification. This specific combined process can achieve high 1,3-isomer selectivity, high fluorination conversion, low
aldehyde byproduct levels, and good long-term
continuous operation stability without separating the cyclization intermediate.