反应详情

In 139 g of methanol was dissolved 46.3 g (0.1 mole) of benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-pivaloyloxypropane-1-sulfonate in Synthesis Example 2. The solution was stirred under ice cooling, to which a solution of 8.0 g (0.2 mole) of sodium hydroxide in 24 g of water was added dropwise at a temperature below 20° C. The solution was stirred overnight at room temperature, after which 21 g of conc. hydrochloric acid and 60 g of water were added to quench the reaction. Methanol was removed in vacuum from the reaction solution, dichloromethane and water were added to the residue, and the organic layer was separated and concentrated again. To the residue containing some white crystals, 150 g of diisopropyl ether was added for crystallization. Filtration and drying gave the target compound. White crystals, 37 g, yield 98%.

1. customin Synthesis Example 2
2. additionwas added dropwise at a temperature below 20° C
3. customto quench
4. customthe reaction
5. customMethanol was removed in vacuum from the reaction solution, dichloromethane and water
6. additionwere added to the residue
7. customthe organic layer was separated
8. concentrationconcentrated again
9. additionTo the residue containing some white crystals, 150 g of diisopropyl ether
10. additionwas added for crystallization
11. filtrationFiltration
12. customdrying
13. customgave the target compound