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Sodium Hydroxide → 4-benzyloxy-1-(2-fluorobenzenesulfonyl)-1H-indole

HRID 1835914
ノート
印刷プレビュー

反応式

HRID 1835914 の反応式
[CH2:1]([O:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH:11]=[CH:12][NH:13]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].[F:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[S:27](Cl)(=[O:29])=[O:28]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl>[CH2:1]([O:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH:11]=[CH:12][N:13]2[S:27]([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[F:20])(=[O:29])=[O:28])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 14798Sodium Hydroxide2 回HCID 884654-(phenylmethoxy)-1H-indoleHCID 1377612-Fluorobenzenesulphonyl chloride2 回

生成物 1

HCID 121489984-benzyloxy-1-(2-fluorobenzenesulfonyl)-1H-indole収率 91%

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒
HCID 6344
Dichloromethane
溶媒

実験手順

To a magnetically stirred mixture of 4-benzyloxyindole (13.80 g, 0.062 mol), tetrabutylammonium hydrogen sulfate (1.05 g, 0.0031 mol) and finely ground sodium hydroxide (2.72 g, 0.068 mol) in 100 mL of dichloromethane at 0° C., was added 2-fluorobenzenesulfonyl chloride (13.25 g, 0.068 mol). After 18 hours stirring at ambient temperature, 2-fluorobenzenesulfonyl chloride (3.96 g, 0.020 mol) and finely ground sodium hydroxide (0.82 g, 0.020) were added. One hour later, the reaction mixture was washed sequentially with water (2×100 ML) and an aqueous K2CO3 solution (2 M, 100 mL). The aqueous fractions were combined and extracted with CH2Cl2 (2×45 mL). The organic fractions were combined, dried over MgSO4 and concentrated in vacuo. The resulting solid was recrystallized from 10:2 ethyl acetate/hexanes (100 mL) to give 4-benzyloxy-1-(2-fluorobenzenesulfonyl)-1H-indole as an off-white powder (21.48 g, 91%). MP 117-120° C.

後処理

  1. washOne hour later, the reaction mixture was washed sequentially with water (2×100 ML)
  2. extractionextracted with CH2Cl2 (2×45 mL)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe resulting solid was recrystallized from 10:2 ethyl acetate/hexanes (100 mL)

出典と根拠

ORDレコード
ord-f1877373559348c79650b8eb14559a6f
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06774241B2

反応ノート

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