反应详情

A mixed solution of 18.0 g (0.10 mole) of 2,2-bistrifluoromethyloxylane, 10.4 g (0.10 mole) of sodium hydrogen sulfite, 19.3 g of water, and 0.62 g of 25% sodium hydroxide was stirred at 40° C. for 10 hours to prepare sodium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate. The obtained sodium sulfonate was used in the subsequent reaction without isolation. After sodium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate was prepared, into it were added 290 g (0.10 mole) of the triphenylsulfonium chloride aqueous solution prepared by the method of Synthesis Example 1-1 and 500 g of methylene chloride, and the resulted mixture was stirred at room temperature for 4 hours. After the stirring, the organic layer was separated, washed by water, and then concentrated under reduced pressure. Into the condensed solution was added methyl isobutyl ketone and the resulted mixture was concentrated again under reduced pressure to distil the remaining water out. Into the obtained residue was added diisopropyl ether for recrystallization. The obtained crystals were recovered and dried to obtain the intended triphenylsulfonium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate (40.8 g of white crystals (yield 78%)). The structure of the intended product is shown below.

1. customAfter the stirring, the organic layer was separated
2. washwashed by water
3. concentrationconcentrated under reduced pressure
4. additionInto the condensed solution was added methyl isobutyl ketone
5. concentrationthe resulted mixture was concentrated again under reduced pressure
6. customto distil the remaining water out
7. additionInto the obtained residue was added diisopropyl ether
8. customfor recrystallization
9. customThe obtained crystals were recovered
10. customdried