Hydrogen peroxide water → Sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfonate

HRID 333111

反応式

HRID 333111 の反応式
[F:1][C:2]([F:22])([S:19]([O-:21])=[O:20])[C:3]([F:18])([F:17])[CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]([CH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)=[O:10].[Na+:23].[OH2:24].OO>O.O.[O-][W]([O-])(=O)=O.[Na+].[Na+].O>[F:22][C:2]([F:1])([S:19]([O-:24])(=[O:21])=[O:20])[C:3]([F:18])([F:17])[CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]([CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1)=[O:10].[Na+:23]

参加物

5

反応物 2

HCID 449047Hydrogen peroxide waterHCID 86660544Sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfinate

生成物 1

HCID 86660542Sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfonate収率 224.3%

試薬・触媒・溶媒 2

HCID 150191Sodium Tungstate Dihydrate触媒HCID 962Water溶媒

実験手順

A glass flask equipped with a thermometer, a condenser and a dropping funnel was charged with 10.0 g (10.5 mmol) of sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfinate having a purity of 39% obtained by Comparative Example 1-2, a catalytic amount of sodium tungstate dihydrate, and 10 ml of water, followed by stirring. Then, 2.4 g (21.0 mmol) of 30% hydrogen peroxide water was added dropwise in an ice bath. After terminating the dropping, stirring was continued at room temperature for one hour. The reaction termination was confirmed by 19F NMR. After concentrating the reaction liquid, it was washed with 10 ml of diisopropyl ether, followed by filtration and drying the obtained solid matter. After that, there was obtained as a white-color solid matter 9.1 g (yield 90%, purity 40%) of sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfonate. Upon this, 7% of 6-bromo-5,5,6,6-tetrafluorohexane cyclohexanecarboxylate was produced as a by-product.

後処理

  1. customA glass flask equipped with a thermometer, a condenser and a dropping funnel
  2. customobtained by Comparative Example 1-2
  3. customAfter terminating the dropping
  4. stirringstirring
  5. concentrationAfter concentrating
  6. customthe reaction liquid, it
  7. washwas washed with 10 ml of diisopropyl ether
  8. filtrationfollowed by filtration
  9. customdrying the obtained solid matter

出典と根拠

ORDレコード
ord-6336f07cc5a74b1b8bfbc2dcd52eee33
出典データセット
uspto-grants-2014_11
特許番号
US08877960B2

関連ノート

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