This invention relates to a method for producing 4-amyl-biphenylcarboxylic acid-3-fluoro-4-cyanophenol ester, comprising: amyl-biphenylcarboxylic acid,
thionyl chloride, 3-fluoro-4-cyanophenol,
toluene,
sodium-
hydroxide, and
anhydrous ethyl
alcohol as
raw material, with mole ration as: amyl-biphenylcarboxylic acid 1.05,
thionyl chloride 2.65, 3-fluoro-4-cyanophenol 1,
toluene 3,
sodium-
hydroxide 0.1, and
anhydrous ethyl
alcohol 4.0. The process comprises two steps: (1) use amyl-biphenylcarboxylic acid and
thionyl chloride as
raw material for
acylation reaction and synthesize amyl-bibenzoyl chloride by normal pressure and decreasing pressure
distillation; (2) dropwise add amyl-bibenzoyl chloride and 3-fluoro-4-cyanophenol with
toluene as
solvent for esterification, and produce the target product 4-amyl-biphenylcarboxylic acid-3-fluoro-4-cyanophenol ester by
water washing, alkaline washing,
crystallization and recrystallization, wherein the conditions:
acylation reaction temperature 160Deg C,
reflux time 6h, normal
distillation temperature 172-176Deg C, pressure decreasing temperature 118-121Deg C, vacuum 50mmHg, the discharging condition is to collect the 3Deg C range product after
temperature and pressure stabilized, the temperature of adding 3-fluoro-4-cyanophenol with agitation for
acylation reaction is 100Deg C, keep the temperature between 90 and 100Deg C when dropwise adding amyl-bibenzoyl chloride for 3h,
reflux with agitation for 6h, heating
steam pressure no more than 0.2MPa,
autoclave inside temperature kept at 120+2Deg C,
crystallization temperature -15Deg C and kept at -15+-2Deg C for 1h for agitation, recrystallization temperature -15Deg Cand kept at -15+-2Deg C for 1h for agitation.