反应详情

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 stirring under ice cooling, 54.0 g of a 5% sodium hydroxide aqueous solution was added dropwise to the solution at a temperature below 10° C. The reaction solution 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 under vacuum, and 270 g of dichloromethane was added. The organic layer was washed with 40 g of water three times. The organic layer was then concentrated and 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%).

1. customsynthesized in Synthesis Example 10
2. customto quench
3. customthe reaction
4. distillationThe methanol was distilled off under vacuum, and 270 g of dichloromethane
5. additionwas added
6. washThe organic layer was washed with 40 g of water three times
7. concentrationThe organic layer was then concentrated
8. addition60 g of diethyl ether was added to the residue for crystallization
9. filtrationThe crystals were filtered
10. customdried
11. customobtaining the target compound