Hydrochloric Acid → Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate

HRID 571156노트

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HRID 571156 반응식
Br[C:2]([F:10])([F:9])[C:3]([F:8])([F:7])[CH2:4][CH2:5][OH:6].[S:11](S([O-])=O)([O-:13])=[O:12].[Na+].[Na+].[CH2:19]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[CH3:20].Cl>O.C(#N)C>[F:9][C:2]([F:10])([S:11]([O-:13])=[O:12])[C:3]([F:8])([F:7])[CH2:4][CH2:5][OH:6].[CH2:19]([NH+:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[CH3:20]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 24489Sodium DithioniteHCID 27363694-Bromo-3,3,4,4-tetrafluorobutan-1-ol

생성물 1

HCID 86660801Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate수율 88%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

A 1 L reactor was charged with 100.0 g (0.44 mole/1.0 equivalent) of 4-bromo-3,3,4,4-tetrafluorobutan-1-ol, 300 g of acetonitrile, 250 g of water, 108.2 g (0.62 mole/1.4 equivalent) of sodium dithionite and 53.4 g (0.52 mole/1.2 equivalents) of triethylamine, followed by 4 hours of stirring at 60° C. Upon confirming the termination of the reaction, the reaction liquid underwent cooling and 100 mL of 1N HCl was added thereto, followed by stirring. Subsequently, an organic layer was separated, and then the organic layer was subjected to distillation of the solvent, thereby obtaining 264 g of a target triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate. It exhibited a purity of 46% and a yield of 88% at this time.

후처리

  1. customthe termination of the reaction
  2. customthe reaction liquid underwent
  3. temperaturecooling
  4. stirringby stirring
  5. customSubsequently, an organic layer was separated
  6. distillationthe organic layer was subjected to distillation of the solvent

출처 및 근거

ORD 기록
ord-96823f07e58c450b88a404b7464c34ba
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09024058B2

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