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Sodium hydride → 1-(4'-Ethoxy-2',3'-Difluorophenyl)Methyloxy-2,2,3,3-Tetrafluoro-4-n-Propylbicyclo[2.2.2]octane

HRID 1644130
ノート
印刷プレビュー

反応式

HRID 1644130 の反応式
[F:1][C:2]1([F:16])[C:7]([F:9])([F:8])[C:6]2([CH2:12][CH2:13][CH3:14])[CH2:10][CH2:11][C:3]1([OH:15])[CH2:4][CH2:5]2.Br[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH3:27])=[C:21]([F:28])[C:20]=1[F:29].[H-].[Na+].[Cl-].[NH4+]>CN(C)C=O>[CH2:26]([O:25][C:22]1[CH:23]=[CH:24][C:19]([CH2:18][O:15][C:3]23[CH2:4][CH2:5][C:6]([CH2:12][CH2:13][CH3:14])([CH2:10][CH2:11]2)[C:7]([F:9])([F:8])[C:2]3([F:16])[F:1])=[C:20]([F:29])[C:21]=1[F:28])[CH3:27]
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 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 229135944-Ethoxy-2,3-difluorobenzyl bromideHCID 594809982,2,3,3-Tetrafluoro-1-Hydroxy-4-n-Propylbicyclo[2.2.2]octane

生成物 1

HCID 594809461-(4'-Ethoxy-2',3'-Difluorophenyl)Methyloxy-2,2,3,3-Tetrafluoro-4-n-Propylbicyclo[2.2.2]octane

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

2,2,3,3-Tetrafluoro-1-hydroxy-4-n-propylbicyclo[2.2.2]octane (12) (0.15 g), and 4-bromomethyl-1-ethoxy-2,3-difluorobenzene (5) (0.31 g) were added to a dimethyl formamide suspension (2.0 mL) of sodium hydride (18 mg), the mixture was stirred at room temperature for 6 hours, and then added with saturated aqueous ammonium chloride solution to thereby terminate the reaction. The organic layer was extracted three times with ethyl acetate, the organic layers were combined, and washed with saturated sodium chloride solution. The organic layer was dried over anhydrous sodium sulfate, and the solvent was vaporized off under reduced pressure to thereby obtain a crude product. The crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9:1), to thereby obtain 1-(4′-ethoxy-2′,3′-difluorophenyl)methyloxy-2,2,3,3-tetrafluoro-4-n-propyl bicyclo[2.2.2]octane (13) (yield=0.15 g, yield ratio=58%) as a colorless clear crystal.

後処理

  1. customto thereby terminate
  2. customthe reaction
  3. extractionThe organic layer was extracted three times with ethyl acetate
  4. washwashed with saturated sodium chloride solution
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate

出典と根拠

ORDレコード
ord-3b4a6ef40b9946229829eaacf385dd71
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08124196B2

反応ノート

読み込み中…

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