反应详情

Under the nitrogen gas atmosphere, chloro sulfuric acid is diluted by adding chloro sulfuric acid (21.184 mmol) into methylene chloride (40 ml), and biphenyl (6.168 g, 40.00 mmol) is added gradually into a container in which diluted chloro sulfuric acid is contained keeping the temperature at 0° C., then stirred at the room temperature for 6 hours. The obtained reacted mixture is poured into brine, and deposited white insoluble is removed by suction filtration. Since the small amount of product is possible to be remained, the residue is washed well by methylene chloride. Then the filtrate is extracted by methylene chloride (150 ml×3), and the separated organic phase is dried up using magnesium sulfate. Solvent is vaporized off under vacuum condition, and the obtained crude product is isolated by a column chromatography (φ=50 mm, h=100 mm×2; CH2Cl2), further refined by recrystallization (CHCl3) and 4,4′-biphenyldisulfonylchloride is obtained as a colorless crystal (8.201 g, 23.349 mmol, 58%) (compound A).

1. customat 0° C.
2. customThe obtained reacted mixture
3. customdeposited white insoluble is removed by suction filtration
4. washthe residue is washed well by methylene chloride
5. extractionThen the filtrate is extracted by methylene chloride (150 ml×3)
6. customthe separated organic phase is dried up
7. customthe obtained crude product