反応 #2195486

反応方程式

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

収率 43.0%

溶媒

water

反応条件

後処理

1. 1
   その他at 85° C.
2. 2
   その他for 65 hours
3. 3
   温度to cool
4. 4
   その他to separate a water layer
5. 5
   workup.ADDITIONA saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals
6. 6
   ろ過The crystals were collected by filtration
7. 7
   洗浄washed with a small volume of saturated sodium chloride aqueous solution
8. 8
   その他dried in vacuum

実験手順

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. The reaction took place at 85° C. for 65 hours. The reaction solution was allowed to cool. 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%).

出典