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Tetrabutylammonium Fluoride → N-{4'-Fluoro-2'-[(R)-1-hydroxyethyl]-1,1'-biphenyl-2-yl}-4-methoxybenzenesulfonamide

HRID 2224621
ノート
印刷プレビュー

反応式

HRID 2224621 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N:14](COCC[Si](C)(C)C)[S:15]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)(=[O:17])=[O:16])=[C:4]([C@H:34]([OH:36])[CH3:35])[CH:3]=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH:14][S:15]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)(=[O:16])=[O:17])=[C:4]([C@H:34]([OH:36])[CH3:35])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 69254268N-{4'-Fluoro-2'-[(R)-1-hydroxyethyl]-1,1'-biphenyl-2-yl}-4-methoxy-N-{[2-(trimethylsilyl)ethoxy]methyl}benzenesulfonamide

生成物 1

HCID 69253499N-{4'-Fluoro-2'-[(R)-1-hydroxyethyl]-1,1'-biphenyl-2-yl}-4-methoxybenzenesulfonamide収率 66%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

N-{4′-Fluoro-2′-[(R)-1-hydroxyethyl]-1,1′-biphenyl-2-yl }-4-methoxy-N-{[2-(trimethylsilyl)ethoxy]methyl}benzenesulfonamide (0.28 g, 0.51 mmol) was dissolved in tetrahydrofuran (10 mL) and tetrabutylammonium fluoride in tetrahydrofuran (1.0 M, 0.76 mL, 0.76 mmol) was added. The solution was heated at reflux for six hours. The solution was concentrated in vacuo and the mixture was dissolved in ethyl acetate and washed with water. The solution was dried over anhydrous magnesium sulfate and the solvent was removed in vacuo. The product was passed through a silica gel plug (5:1 hexane: ethyl acetate followed by 1:1 hexane:ethyl acetate) to yield the title compound as a solid (0.135 g, 66% ), m.p. 137-138° C. The NM spectrum of the title compound was consistent with rotamers. The peaks attributed to individual rotamers in the 1H NMR spectrum coalesced at 90° C.

後処理

  1. temperatureThe solution was heated
  2. temperatureat reflux for six hours
  3. concentrationThe solution was concentrated in vacuo
  4. dissolutionthe mixture was dissolved in ethyl acetate
  5. washwashed with water
  6. dry with materialThe solution was dried over anhydrous magnesium sulfate
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-8bd3ed02c7c04cb799ad8a5cb7cceef3
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07378427B2

反応ノート

読み込み中…

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