反应详情

温度

40 °C

A 500 mL reactor was charged with 112 g (46% purity, 0.17 moles) of triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate, 200 g of water and 41 g (0.36 mole) of 30% hydrogen peroxide, at room temperature, followed by 6 hours of stirring at 40° C. Upon confirming the termination of the reaction, a reaction liquid underwent cooling and 7.5 g of sodium sulfite was added to the reaction liquid, followed by stirring. Subsequently, a liquid obtained by distilling the solvent out of the reaction liquid was rinsed with 50 g of hexane, and then extracted with 100 g of chloroform. It was heated under a reduced pressure so as to distill a volatile component off and then dried, thereby obtaining 43 g of a target triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonate. It exhibited a purity of 50% and a yield of 40% at this time. As a result of analysis, it was found that 4-bromo-3,3,4,4-tetrafluorobutan-1-ol which had been confirmed to disappear by the 1st step (sulfination step) was formed during this 2nd step (oxidation step) as a by-product in an amount of 9%.

1. customthe termination of the reaction
2. customa reaction liquid underwent
3. temperaturecooling
4. stirringby stirring
5. customSubsequently, a liquid obtained
6. distillationby distilling the solvent
7. customout of the reaction liquid
8. washwas rinsed with 50 g of hexane
9. extractionextracted with 100 g of chloroform
10. temperatureIt was heated under a reduced pressure so as
11. distillationto distill a volatile component off and
12. customthen dried