2-Chloro-5-iodobenzotrifluoride

liquid

The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF.Phosphorus oxychloride (10.5 mmol) was then added and the system was placed under microwave atmosphere and heated to 130 ° C for 1 hour. After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. The petroleum ether was used as an eluent and flash column chromatography to give 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene as a solid powder, yield 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF, then phosphorus oxychloride (10.5 mmol) was added, and the system was placed in a microwave environment and heated to 130 ° C. , the reaction was 1 hour. After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. The petroleum ether was used as an eluent and flash column chromatography to give 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene as a solid powder, yield 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF.Then add phosphorus oxychloride (10.5 mmol), Put the system in a microwave environment, Heat to 130 ° C and react for 1 hour.After the reaction is completed, the system is cooled to room temperature.Add 30 ml of water to it and stir for 10 minutes.Add 30 ml of dichloromethane and extract.The organic phase was dried over anhydrous sodium sulfate and filtered.The filtrate is distilled off under reduced pressure.The residue uses petroleum ether as the eluent, Rapid column chromatography separation, A solid powder of 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene was obtained in a yield of 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF, then phosphorus oxychloride (10.5 mmol) was added, and the system was placed in a microwave environment and heated to 130 ° C, the reaction was 1 hour. After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. The petroleum ether was used as an eluent and flash column chromatography to give 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene as a solid powder, yield 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF, then phosphorus oxychloride (10.5 mmol) was added, and the system was placed in a microwave environment and heated to 130 ° C. , the reaction was 1 hour. After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. Petroleum ether as an eluent, fast column chromatography, A solid powder of 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene was obtained in a yield of 69percentWill get 1.14-iodo-2-trifluoromethylphenol (10 mmol) was dissolved in 20 ml of DMF.Then add phosphorus oxychloride (10.5 mmol) and place the system in a microwave environment.Heat to 130 ° C, The reaction was for 1 hour.After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes.After adding 30 ml of dichloromethane, the organic phase was dried over anhydrous sodium sulfate and filtered.The residue was purified by column chromatography using petroleum ether as eluent.Yellow 1-chloro-4-iodo-2-trifluoromethylbenzene solid powder, yield 69percentThe 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF, then phosphorus oxychloride (10.5 mmol) was added, and the system was placed in a microwave environment and heated to 130 ° C. , the reaction was 1 hour. After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. The petroleum ether was used as an eluent and flash column chromatography to give 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene as a solid powder, yield 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF, then phosphorus oxychloride (10.5 mmol) was added, and the system was placed in a microwave environment and heated to 130 ° C. , the reaction was 1 hour.After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. Petroleum ether as an eluent, fast column chromatography, A solid powder of 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene was obtained in a yield of 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF.Then add phosphorus oxychloride (10.5 mmol) and place the system in a microwave environment.Heat to 130 ° C and react for 1 hour. After the reaction is completed, the system is cooled to room temperature.30 ml of water was added thereto, stirred for 10 minutes, and then extracted with 30 ml of dichloromethane.The organic phase was dried over anhydrous sodium sulfate, filtered, and then evaporated and evaporated.The residue was separated by flash column chromatography using petroleum ether as eluent.A solid powder of 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene was obtained in a yield of 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF.Then add phosphorus oxychloride (10.5 mmol) and place the system in a microwave environment.Heat to 130 ° C and react for 1 hour.After the reaction was completed, the system was cooled to room temperature, 30 ml of water was added thereto, and the mixture was stirred for 10 minutes, and then extracted with 30 ml of dichloromethane, and the organic phase was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure. Petroleum ether as an eluent, fast column chromatography, Obtaining 2.1 g of a pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene solid powder, The yield was 69percent.The 4-iodo-2-trifluoromethylphenol (10 mmol) obtained in 1.1 was dissolved in 20 ml of DMF.Then add phosphorus oxychloride (10.5 mmol) and place the system in a microwave environment.Heat to 130 ° C and react for 1 hour. After the reaction is completed, the system is cooled to room temperature.Add 30 ml of water to it and stir for 10 minutes.It was extracted with 30 ml of dichloromethane and the organic phase was dried over anhydrous sodium sulfate.Filtration, evaporation of the solvent under reduced pressure, and the residue using petroleum ether as eluent.Flash column chromatography gave 2.1 g of pale yellow 1-chloro-4-iodo-2-trifluoromethylbenzene as a solid powder.The yield was 69percent.

Molecular Weight:306.45
XLogP3:4.1
Hydrogen Bond Acceptor Count:3
Exact Mass:305.89201
Monoisotopic Mass:305.89201
Heavy Atom Count:12
Complexity:159
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes