4-Bromo-4'-iodobiphenyl synthesis
- Product Name:4-Bromo-4'-iodobiphenyl
- CAS Number:105946-82-5
- Molecular formula:C12H8BrI
- Molecular Weight:359
92-66-0
105946-82-5
Under argon protection, 4-bromobiphenyl (47.0 g, 201.6 mmol), iodine (23.0 g, 90.6 mmol) and disodium hydriodate (9.4 g, 41.2 mmol) were added sequentially to the reaction flask. Subsequently, water (42 mL), acetic acid (360 mL) and sulfuric acid (11 mL) were added to the reaction system. The reaction mixture was heated to 65 °C and stirred at this temperature for 30 min. Then, the temperature was raised to 90 °C and the reaction continued to be stirred for 6 hours. Upon completion of the reaction, the reaction mixture was slowly poured into ice water to precipitate a solid. The solid product was collected by filtration and washed sequentially with water and methanol to give a final white solid 4-bromo-4'-iodobiphenyl (67.0 g, 93% yield).
92-66-0
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105946-82-5
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Yield:105946-82-5 93%
Reaction Conditions:
with periodic acid dihydrate;sulfuric acid;iodine;acetic acid at 65 - 90; for 6.5 h;Inert atmosphere;
Steps:
synthesis of intermediate 1-4 (intermediate 1-4)
Under argon atmosphere, were weighed 4-bromo-biphenyl 47. 0g (201. 6mmol), iodine 23. 0g (90. 6mmol), periodic acid dihydrate 9. 4g (41. 2mmol), water was added 42ml, 360ml acetic acid, 11 ml of sulfuric acid, 65 ° C with stirring for 30 minutes, to 90 ° C and further stirred for 6 hours.After the reaction, the reaction mixture after injected into to the ice water, filtered. After washing with water, further washed with methanol, thereby obtaining 67.0g white solid (yield 93%).
References:
CN105431417,2016,A Location in patent:Paragraph 0214; 0215; 0216; 0217
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