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 1-10. 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 allowed to mature 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, and 60 g of diethyl ether was added to the concentrate for crystallization. The crystals were filtered and dried, obtaining the target compound. White crystals, 24.3 g (yield 85%).

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