3,4,5-TRIFLUOROBENZOTRIFLUORIDE

Preparation method of 3, 4, 5-trifluorobenzotrifluoride; 860 g of dry sulpholane and 524 g of dry KF were initially charged with exclusion of moisture in an autoclave, and 500 g of 3, 4, 5-trichlorobenzotrifluoride, 5 g of nitrobenzene and 25 g of CNC catalyst were added. The vessel was sealed and the mixture subsequently heated to 200° C. for 5 h and then to 220° C. for a further 12 h. During the reaction, a maximum total pressure of 9 bar arose. The mixture was then cooled to 20° C. and decompressed into a cooled receiver. The product was distilled off at standard pressure. After redistillation of the crude product, 300 g of 3, 4, 5-trifluorobenzotrifluoride (75percent of theory) were obtained as a colourless liquid.Preparation method of 3, 4, 5-trifluorobenzotrifluoride; 860 g of dry sulpholane and 524 g of dry KF were initially charged with exclusion of moisture in an autoclave, and 500 g of 3, 4, 5-trichlorobenzotrifluoride, 5 g of nitrobenzene and 25 g of CNC catalyst were added. The vessel was sealed and the mixture subsequently heated to 200° C. for 5 h and then to 220° C. for a further 12 h. During the reaction, a maximum total pressure of 9 bar arose. The mixture was then cooled to 20° C. and decompressed into a cooled receiver. The product was distilled off at standard pressure. After redistillation of the crude product, 300 g of 3, 4, 5-trifluorobenzotrifluoride (75percent of theory) were obtained as a colourless liquid.Synthesis Example 27 N-{1-[2, 6-Difluoro-4-(trifluoromethyl)phenyl]-1H-pyrazol-3-yl}-2-(trifluoromethyl)benzamide (Compound (I-1-230) in Table 1) Analogously to Synthesis Example 25, Step 2, starting with Sodium hydride (17 mg) was added to a solution of 3-chloro-4-[5-[1-hydroxy-1-methylethyl]-4-methyl-4H-1, 2, 4-triazol-3-yl}benzonitrile(100 mg) in DMF (1 ml) under ice cooling, followed by stirring at the same temperature for 10 minutes, and 3, 4, 5-trifluorobenzenotrifluoride (87 mg) was added thereto, followed by stirring in an ice bath for 3 hours. Water was added to the reaction mixture to cease the reaction followed by extraction with ethyl acetate. The organic layer was washed with water twice, then washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol:chloroform=100:0 to 100:2). The residue was powdered in diethylether, collected by filtration and washed with diethylether. The resulting powder was suspended in ethanol, an aqueous hydrogen peroxide solution (86 mul) and a 1M aqueous sodium hydroxide solution (0.4 ml) were sequentially added thereto under ice cooling, followed by stirring at room temperature for 2 hours. Water and ethyl acetate were added thereto with ice-cooling to perform separation operation. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was concentrated under reduced pressure. The residue was purified by silica gel column chromatography, and then by thin layer chromatography, powdered in diethylether and then collected by filtration to obtain 3-chloro-4-(5-{1-[2, 6-difluoro-4-(trifluoromethyl)phenoxy]-1-methylethyl}-4-methyl-4H-1, 2, 4-triazol-3-yl}benzamide (45.7 mg), as a white powder.EXAMPLE 6 This Example illustrates the preparation of 3-(2, 6-difluoro-4-trifluoromethylphenoxy)benzoic acid by the process of claim 1. A solution of 3-hydroxybenzoic acid (5.5 g) and EXAMPLE V Preparation of: 3-carbomethoxymethyl-5-(2, 6-difluoro-4-trifluoromethylphenoxy) benzoxazolone A mixture of 1.33 grams (0.006 mole) of 3-carbomethoxymethyl-5-hydroxybenzoxazolone, 1.32 grams (0.0066 mole) of This Example illustrates the preparation of 1-(2, 6-difluoro-4-trifluoromethylphenyl)-4-trifluoromethyl -2-pyridone (Compound No. 20, Table I). A well stirred mixture of 4-trifluoromethyl-2-pyridone (1.5 g, 9.2 mmol), Example IV-4 In a stainless steel autoclave, 500 g of EXAMPLE 3 500 g of 1-Cyclopropyl-7, 8-difluoro-5-trifluoromethyl-1, 4-dihydro-4-oxo-3-quinolinecarboxylic acid STR88 a) 2, 3, 4-Trifluoro-6-trifluoromethylbenzoic acid The title compound is obtained when Preparation method of

Molecular Weight:200.08
XLogP3:3.1
Hydrogen Bond Acceptor Count:6
Exact Mass:200.00606904
Monoisotopic Mass:200.00606904
Heavy Atom Count:13
Complexity:164
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes