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ChemicalBook CAS DataBase List 2-BROMO-1-FLUORO-3-IODOBENZENE

2-BROMO-1-FLUORO-3-IODOBENZENE synthesis

5synthesis methods
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Yield: 80%

Reaction Conditions:

Stage #1:2-bromo-3-fluoroaniline with sulfuric acid;sodium nitrite in water at 20; for 3 h;
Stage #2: with potassium iodide in water for 4 h;

Steps:

1.3 3. Preparation of 1-fluoro-2-bromo-3-iodobenzene
Under mechanical stirring, slowly add 44.8 g of water to the 250 mL glass reaction bottle.Concentrated sulfuric acid was 32.0 g and 1-fluoro-2-bromo-3-aminobenzene was 14.9 g.A solution of 5.9 g of sodium nitrite and 11.8 g of water was added dropwise at room temperature, and the mixture was dripped in about 2 hours.Stirring was continued for 1 hour at room temperature. A solution of 15.0 g of potassium iodide and 21.5 g of water was added dropwise at room temperature.After about 2 hours, the stirring was continued for 2 hours at room temperature. The reaction solution was extracted with 29.8 g of dichloromethane.The oil layer was respectively treated with 5% sodium sulfite aqueous solution 35.0 g,35.0 g of a 5% aqueous sodium hydroxide solution and 35.0 g of water were washed successively, and the solvent was concentrated.Distilled under reduced pressure1-Fluoro-2-bromo-3-iodobenzene 18.9 g, yield 80%.

References:

Jinkai (Liaoning) Chemical Co., Ltd.;Li Zhenwei;Zhao Yang;Li Degang;Liu Shukuan;Jiang Zhipeng;Liu Haisheng;Wang Dong;Zhao Hongyang;Song Tongji CN108002976, 2018, A Location in patent:Paragraph 0045; 0047; 0052; 0053; 0062; 0071