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Perfluoro-1-butanesulfonyl fluoride → HCID 86674269、化合物

HRID 405198
ノート
印刷プレビュー

反応式

HRID 405198 の反応式
CC([O-])(C)C.[K+].[Cl:7][C:8]1[C:9]([C:17]([F:20])([F:19])[F:18])=[CH:10][C:11]([OH:16])=[C:12]([CH:15]=1)[CH:13]=[O:14].[F:21][C:22]([F:37])([S:33](F)(=[O:35])=[O:34])[C:23]([F:32])([F:31])[C:24]([F:30])([F:29])[C:25]([F:28])([F:27])[F:26]>C1COCC1>[F:37][C:22]([F:21])([S:33]([O:16][C:11]1[CH:10]=[C:9]([C:17]([F:18])([F:19])[F:20])[C:8]([Cl:7])=[CH:15][C:12]=1[CH:13]=[O:14])(=[O:35])=[O:34])[C:23]([F:31])([F:32])[C:24]([F:30])([F:29])[C:25]([F:28])([F:27])[F:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 67814Perfluoro-1-butanesulfonyl fluorideHCID 23665647Potassium tert-butoxideHCID 86674268HCID 86674268、化合物

生成物 1

HCID 86674269HCID 86674269、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A 1.04 M THF solution of t-BuOK (4.9 mL, 5.1 mmol) was added to a 0° C., THF solution (4 mL) of 5-chloro-2-hydroxy-4-(trifluoromethyl)benzaldehyde (1.0 g, 4.6 mmol). After 4 min, neat 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride (1.7 mL, 9.3 mmol) was added and the ice bath was removed. After 1 h at room temperature, AcOH (1 mL) was added and the resulting mixture was concentrated. The resulting material was diluted with DCM and 1M aqueous HCl, the layers were separated, and the organic layer was washed with 1 M NaHCO3, dried (Na2SO4), and concentrated to yield the title compound that was used without further purification.

後処理

  1. customthe ice bath was removed
  2. waitAfter 1 h at room temperature
  3. additionAcOH (1 mL) was added
  4. concentrationthe resulting mixture was concentrated
  5. additionThe resulting material was diluted with DCM and 1M aqueous HCl
  6. customthe layers were separated
  7. washthe organic layer was washed with 1 M NaHCO3
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-2201bf8f26e44e1790dc8ce1c220b374
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08748624B2

反応ノート

読み込み中…

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