反应详情

温度

80 °C

9.3 g of 2,2-difluoroethenyl tosylate, which had been synthesized by a conventional technique, was dispersed in 17 g of water and 37 g of methanol, after which 4.7 g of sodium hydrogen sulfite and 0.5 g of benzoyl peroxide were added. The reaction mixture was stirred at 80° C. for 40 hours. The reaction solution was allowed to cool, after which methanol was distilled off in vacuum. Toluene was added, followed by separatory operation to separate a water layer. A saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals settled out. The crystals were collected by filtration, washed with a small volume of saturated sodium chloride aqueous solution and then dried in vacuum, obtaining the target compound, sodium 1,1-difluoro-2-tosyloxyethanesulfonate. White crystals, 2.5 g (yield 16%).

1. temperatureto cool
2. distillationafter which methanol was distilled off in vacuum
3. additionToluene was added
4. customto separate a water layer
5. additionA saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals
6. filtrationThe crystals were collected by filtration
7. washwashed with a small volume of saturated sodium chloride aqueous solution
8. customdried in vacuum