Water → HCID 86632756、化合物

HRID 405012

反応式

HRID 405012 の反応式
[OH:1][CH2:2][C:3]([F:9])([F:8])[S:4]([OH:7])(=[O:6])=[O:5].[Na].O.[Cl-].[C:13]1([S+:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(Cl)(Cl)Cl>[OH:1][CH2:2][C:3]([F:9])([F:8])[S:4]([O-:7])(=[O:6])=[O:5].[C:26]1([S+:19]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

参加物

5

反応物 3

HCID 962WaterHCID 61343Triphenylsulfonium chloride5 回HCID 86650905HCID 86650905、化合物2 回

生成物 1

HCID 86632756HCID 86632756、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A 2 L reactor was charged with 183.7 g (38% purity, 0.38 mole) of sodium 2-hydroxy-1,1-difluoroethanesulfonic acid, 300 mL of water, 450 mL of chloroform and an aqueous solution of triphenylsulfonium chloride [142.8 g (0.49 mole/1.25 equivalents) of triphenylsulfonium chloride and 150 mL of water], followed by stirring at room temperature for 1 hour. A reaction solution was analyzed by using nuclear magnetic resonance (NMR), by which there was found almost half the raw material sodium 2-hydroxy-1,1-difluoroethanesulfonic acid remaining. Accordingly, the reactor was further charged with the aqueous solution of triphenylsulfonium chloride [142.8 g (0.49 mole/1.25 equivalents) of triphenylsulfonium chloride and 150 mL of water], followed by stirring at room temperature for 0.5 hour (triphenylsulfonium chloride was used in an amount of 285.7 g (0.96 mole/2.5 equivalents) in total and the reaction time was 1.5 hours in total). The reaction solution was analyzed by using nuclear magnetic resonance (NMR), by which the raw material was detected being consumed. Thereafter, the reaction solution was separated. The obtained water layer was extracted with 100 mL of chloroform three times while distilling a solvent out of the obtained organic layer, thereby obtaining 328.2 g of the target triphenylsulfonium 2-hydroxy-1,1-difluoroethanesulfonate. In this case, the purity was 48% and the yield was 97%.

後処理

  1. waitthe reaction time was 1.5 hours
  2. customby which the raw material was detected being consumed
  3. customThereafter, the reaction solution was separated
  4. extractionThe obtained water layer was extracted with 100 mL of chloroform three times
  5. distillationwhile distilling a solvent out of the obtained organic layer

出典と根拠

ORDレコード
ord-7d525ea3ae0e4186b6f58d6de61ff2e1
出典データセット
uspto-grants-2014_06
特許番号
US08748672B2

関連ノート

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