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

HRID 571156

反応式

HRID 571156 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-96823f07e58c450b88a404b7464c34ba
出典データセット
uspto-grants-2015_05
特許番号
US09024058B2

関連ノート

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