반응 #2161237

반응 방정식

toluene

1,1,3,3,3-pentafluoropropen-2-yl benzoate

sodium hydrogen sulfite

benzoyl peroxide

→

sodium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate

수율 43.0%

용매

water

반응 조건

후처리

1. 1
   기타Reaction
2. 2
   온도to cool
3. 3
   기타to separate a water layer
4. 4
   workup.ADDITIONA saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals
5. 5
   여과The crystals were collected by filtration
6. 6
   세척washed with a small volume of saturated sodium chloride aqueous solution
7. 7
   기타dried in vacuum

실험 절차

10.0 g of 1,1,3,3,3-pentafluoropropen-2-yl benzoate which had been synthesized by a conventional technique, was dispersed in 72 g of water, after which 12.0 g of sodium hydrogen sulfite and 1.24 g of benzoyl peroxide were added. Reaction occurred at 85° C. for 65 hours. The reaction solution was allowed to cool, after which 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 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate. White crystals, 5.85 g (yield 43%).

출처