3-Chloro-4-fluorobenzotrifluoride

Clear colorless liquid

In a 500 ml four-necked flask equipped with a condenser, 200 mL of DMA, 0.2 mol of 3, 4-Dichloro-trifluorotoluene, 1.0mol potassium fluoride, 0.01mol tetraphenylphosphine chloride, 150 incubated to the material 3, 4-dichloro-benzotrichloride gas content of less than 1percent, filtered by suction Potassium fluoride and catalyst recovery, applied to the next batch; the mother liquor was dissolved, the content of the rectification was 99percent of 3-chloro-4-fluoro-trifluoromethyl toluene, Yield 90percent;In the same manner as in Example 8, the compound 45 was obtained as N-(2-((1-(4-chlorophenyl)-1H-pyrazol-3-yl)oxy)phenyl)-2-(4) -Hydroxyphenyl)amide, and then compound 51 is prepared by the following reaction:N-(2-((1-(4-chlorophenyl)-1H-pyrazol-3-yl)oxy)phenyl)-2-(4-hydroxyphenyl)amide was added sequentially to the reaction flask ( 0.34 g, 0.86 mmol), DMF (5 mL), 3-chloro-4-fluorotrifluoromethylbenzene (0.21 g, 1.04 mmol) and potassium carbonate (0.10 g, 1.04 mmol), The reaction solution was heated to reflux. After refluxing for 2 hours, The reaction mixture was poured into water (50 ml).The organic layer was washed with brine (50 ml)The residue was purified by column chromatography (as eluent PE: EA = 10: 1) to give 0.41 g yellow solid, yield 78.76%.The cyanation reaction adds a certain amount of DMF to the reactor.Sodium cyanide solution and4-fluoro-3-chlorobenzotrifluorideIn equimolar amounts, Catalyst tetrabutylammonium chloride, Drop added4-fluoro-3-chlorobenzotrifluorideRaise the temperature to 110-115C and reflux the reaction for 3 hours.After passing the sampling, steam distillation distills intermediate 1Mother liquor recovery DMF application.Among them, the intermediate 1 is C8H3ClF3N, the product is C8H3ClF3N and sodium fluoride NaF;In a 500 ml four-necked flask equipped with a condenser, 200 mL of DMA, 0.6 mol of 5.00 g (45.82 mmol) of 2-aminophenol and 9.10 g (45.82 mmol) of 5.00 g (45.82 mmol) of 2-aminophenol and 9.10 g (45.82 mmol)5.00 g (45.82 mmol) of 2-aminophenol and 9.10 g (45.82 mmol) of General procedure: 3 mmol of 1-chloro-4-trifluorotoluene, 3.3 mmol of 2-aminophenol of formula I-4 and 3.6 mmol of potassium carbonate were added to a 50 mL round bottom flask, 20 mL of DMF was added, and the temperature was raised to 70C. TLC monitored the reaction of the starting material and stopped the reaction. 50 mL of ethyl acetate was added, and each was washed twice with 50 mL of saturated brine and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and subjected to column chromatography to obtain Formula 3 (II-2). The indicated compound (yield 70%).In a 500 ml four-necked flask equipped with a condenser, 200 mL of DMA, 0.2 mol of 3, 4-Dichloro-trifluorotoluene, 1.0mol potassium fluoride, 0.01mol tetraphenylphosphine chloride, 150 incubated to the material 3, 4-dichloro-benzotrichloride gas content of less than 1%, filtered by suction Potassium fluoride and catalyst recovery, applied to the next batch; the mother liquor was dissolved, the content of the rectification was 99% of 3-chloro-4-fluoro-trifluoromethyl toluene, Yield 90%;

Used as medicine and pesticide intermediate

Molecular Weight:198.54
XLogP3:3.5
Hydrogen Bond Acceptor Count:4
Exact Mass:197.9859404
Monoisotopic Mass:197.9859404
Heavy Atom Count:12
Complexity:156
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes