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ChemicalBook CAS DataBase List 1-Chloro-4-(difluoroMethyl)benzene, 97%

1-Chloro-4-(difluoroMethyl)benzene, 97% synthesis

8synthesis methods
-

Yield:43141-66-8 96.08%

Reaction Conditions:

with hydrogen fluoride;antimony(III) chloride at 120; for 4 h;Autoclave;Temperature;

Steps:

3 Example 3: Preparation of 1-chloro-4-(difluoromethyl)benzene

P-chlorobendichloride 97.75g (0.5mol)And antimony trichloride 0.7g (0.025mol)Mix well in the autoclave,Reduce the pressure to remove the air in the kettle,Pump 100g (5.0mol) of hydrogen fluoride gas at room temperature,Warm up to 120°C and react for 4h,Cool to 40°C,Exhaust and collect the gas in the kettle,And blow it clean with nitrogen (200g, 7.14mol),Through cryogenic cooling,Cool the HF to liquid,The remaining gas is absorbed by water,Prepared into hydrochloric acid solution.The remaining mixture in the kettle was distilled under reduced pressure to get the product 1-chloro-4-(difluoromethyl)benzene,Collect the fractions under 6065/2.4Kpa,The product was liquefied by cooling to obtain a colorless liquid (78.05g, 0.481mol),The yield is 96.08% (calculated on the basis of p-chlorobendichloride),The chromatographic purity is 99.80%.

References:

CN113185473,2021,A Location in patent:Paragraph 0016; 0022-0028