Hydrogen Peroxide → Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonate

HRID 571157노트

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HRID 571157 반응식
[F:1][C:2]([F:12])([S:9]([O-:11])=[O:10])[C:3]([F:8])([F:7])[CH2:4][CH2:5][OH:6].[CH2:13]([NH+:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH3:14].O.OO.S([O-])([O-])=[O:24].[Na+].[Na+]>CC(C)=O>[F:12][C:2]([F:1])([S:9]([O-:24])(=[O:11])=[O:10])[C:3]([F:7])([F:8])[CH2:4][CH2:5][OH:6].[CH2:13]([NH+:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH3:14]

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 962WaterHCID 24437Sodium SulfiteHCID 86660801Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate

생성물 1

HCID 86660802Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonate수율 95%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
40 °C

실험 절차

A 500 mL reactor was charged with 65 g (93% purity, 0.194 mole/1.0 equivalent) of triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate obtained in Example 2-1 by purification, 200 g of water and 46 g (0.40 mole/2.1 equivalents) of 30% hydrogen peroxide at room temperature, followed by 6 hours of stirring at 40° C. Upon confirming the termination of the reaction, the reaction liquid underwent cooling, and 7.5 g of sodium sulfite was added to the reaction liquid, followed by stirring. Thereafter, 350 g of acetone was added to a liquid obtained by distilling the solvent out of the reaction liquid, followed by 1 hour of stirring at room temperature. Thereafter, filteration was performed in the use of a filter paper. An obtained filtrate was concentrated and dried, thereby obtaining 65.6 g of a target triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonate. It exhibited a purity of 92% and a yield of 95% at this time.

후처리

  1. customthe termination of the reaction
  2. customthe reaction liquid
  3. temperatureunderwent cooling
  4. stirringby stirring
  5. customobtained
  6. distillationby distilling the solvent
  7. customout of the reaction liquid
  8. waitfollowed by 1 hour
  9. stirringof stirring at room temperature
  10. concentrationAn obtained filtrate was concentrated
  11. customdried

출처 및 근거

ORD 기록
ord-08bdf0e2e73e4a8b8d9d67b77e60d302
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09024058B2

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