Hydrochloric Acid → Triphenylsulfonium 4-hydroxy-1,1,2,2-tetrafluorobutanesulfonate

HRID 1662167ノート

反応式

HRID 1662167 の反応式
C([O:9][CH2:10][CH2:11][C:12]([F:21])([F:20])[C:13]([F:19])([F:18])[S:14]([O-:17])(=[O:16])=[O:15])(=O)C1C=CC=CC=1.[C:22]1([S+:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.[OH-].[Na+].Cl>CO>[OH:9][CH2:10][CH2:11][C:12]([F:21])([F:20])[C:13]([F:18])([F:19])[S:14]([O-:17])(=[O:15])=[O:16].[C:35]1([S+:28]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86654882Triphenylsulfonium 4-benzoyloxy-1,1,2,2-tetrafluorobutanesulfonate

生成物 1

HCID 86639888Triphenylsulfonium 4-hydroxy-1,1,2,2-tetrafluorobutanesulfonate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 8 g of methanol was dissolved 2.1 g of triphenylsulfonium 4-benzoyloxy-1,1,2,2-tetrafluorobutanesulfonate synthesized in Synthesis Example 9. The solution was stirred under ice cooling, to which 2.5 g of a 9% sodium hydroxide aqueous solution was added dropwise at a temperature below 10° C. The solution was aged at room temperature for 70 hours, after which 22 g of 1N hydrochloric acid was added under ice cooling for quenching the reaction. The methanol was removed under vacuum. Dichloromethane was added to the organic layer, which was washed three times with water. The organic layer was concentrated and dried, obtaining the target compound. Colorless oily matter, 0.3 g.

後処理

  1. customsynthesized in Synthesis Example 9
  2. additionwas added dropwise at a temperature below 10° C
  3. customfor quenching
  4. customthe reaction
  5. customThe methanol was removed under vacuum
  6. additionDichloromethane was added to the organic layer, which
  7. washwas washed three times with water
  8. concentrationThe organic layer was concentrated
  9. customdried
  10. customobtaining the target compound

出典と根拠

ORDレコード
ord-4453f01272b742c29ad58522509735cc
出典データセット
uspto-grants-2011_10
特許番号
US08030515B2

反応ノート

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