반응 #577231

반응 방정식

sodium hydroxide

triphenylsulfonium 2-benzoyloxy-1,1,3,3,3-pentafluoropropane-1-sulfonate

hydrochloric acid

→

triphenylsulfonium 2-hydroxy-1,1,3,3,3-pentafluoropropane-1-sulfonate

수율 85.0%

용매

methanol

반응 조건

후처리

1. 1
   기타synthesized in Synthesis Example 10
2. 2
   기타to quench
3. 3
   기타the reaction
4. 4
   workup.DISTILLATIONThe methanol was distilled off in vacuum
5. 5
   workup.ADDITIONafter which 270 g of dichloromethane was added to the residue
6. 6
   세척The organic layer was washed with 40 g of water three times
7. 7
   농축The organic layer was concentrated
8. 8
   workup.ADDITIONafter which 60 g of diethyl ether was added to the residue for crystallization
9. 9
   여과The crystals were filtered
10. 10
    기타dried
11. 11
    기타obtaining the target compound

실험 절차

In 72 g of methanol was dissolved 34.4 g of triphenylsulfonium 2-benzoyloxy-1,1,3,3,3-pentafluoropropane-1-sulfonate synthesized in Synthesis Example 10. While the solution was stirred under ice cooling, 54.0 g of 5% sodium hydroxide solution was added dropwise at a temperature below 10° C. It was aged at the temperature for 4 hours. At a temperature below 10° C., 6.8 g of 12N hydrochloric acid was added to quench the reaction. The methanol was distilled off in vacuum, after which 270 g of dichloromethane was added to the residue. The organic layer was washed with 40 g of water three times. The organic layer was concentrated, after which 60 g of diethyl ether was added to the residue for crystallization. The crystals were filtered and dried, obtaining the target compound. White crystals, 24.3 g (yield 85%).

출처