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Sodium → (5-Fluoro-2-phenoxy-phenyl)-(5-methoxy-2-[2-(tosyloxy-)-ethoxy]-benzyl}-amine

HRID 1717516
ノート
印刷プレビュー

反応式

HRID 1717516 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([NH2:8])[CH:7]=1.[CH3:16][O:17][C:18]1[CH:19]=[CH:20][C:21]([O:26][CH2:27][CH2:28][O:29][S:30]([C:33]2[CH:39]=[CH:38][C:36]([CH3:37])=[CH:35][CH:34]=2)(=[O:32])=[O:31])=[C:22]([CH:25]=1)[CH:23]=O.[Na]>ClC(Cl)C.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([NH:8][CH2:23][C:22]2[CH:25]=[C:18]([O:17][CH3:16])[CH:19]=[CH:20][C:21]=2[O:26][CH2:27][CH2:28][O:29][S:30]([C:33]2[CH:34]=[CH:35][C:36]([CH3:37])=[CH:38][CH:39]=2)(=[O:32])=[O:31])[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 5360545SodiumHCID 196271325-Fluoro-2-phenoxyanilineHCID 59765853HCID 59765853、化合物

生成物 1

HCID 86621789(5-Fluoro-2-phenoxy-phenyl)-(5-methoxy-2-[2-(tosyloxy-)-ethoxy]-benzyl}-amine収率 71%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6365
1,1-Dichloroethane
溶媒

実験手順

To stirred solution of 9.1 g (45 mmol) 1b, 15.8 g (45 mmol) 5a and one drop of glacial acid in 60 ml dichloroethane (pH=5) were added 14.8 g (70 mmol) sodium tris-acetoxy hydro borane. The reaction mixture was stirred over night and diluted with 5 ml water. The pH value was adjusted with aqueous sodium hydroxyd solution to pH=8-9. The mixture was extracted three times with dichloromethane. The combined organic phases were washed with water and brine and were dried with magnesium sulfate. The desired crude product 5b was obtained in 71% yield (17.2 g, 32.0 mmol) as yellow oil. The crude product 5b was used without further purification.

後処理

  1. extractionThe mixture was extracted three times with dichloromethane
  2. washThe combined organic phases were washed with water and brine
  3. dry with materialwere dried with magnesium sulfate

出典と根拠

ORDレコード
ord-7be09e1615004a95bd8380c33dda484b
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803960B2

反応ノート

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