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Water → 8-Fluoro-3,4-dihydro-5-methoxy-1(2H)-naphthalenone

HRID 374657
ノート
印刷プレビュー

反応式

HRID 374657 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH3:15])=[C:6]([CH2:8][CH2:9][CH2:10][C:11]([OH:13])=O)[CH:7]=1.O.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH3:15])=[C:6]2[C:7]=1[C:11](=[O:13])[CH2:10][CH2:9][CH2:8]2
参加物反応条件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 962WaterHCID 516892Sodium BicarbonateHCID 118060004-(5-Fluoro-2-methoxyphenyl)butanoic acid

生成物 1

HCID 108563538-Fluoro-3,4-dihydro-5-methoxy-1(2H)-naphthalenone

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

4-(5-Fluoro-2-methoxy phenyl)butanoic acid (15 g) was mixed with polyphosphoric acid (60 g) and stirred with an overhead stirrer. The reaction mixture was heated to 90° C. and stirred at this temperature for 45 minutes. The reaction mixture was allowed to cool, water (100 ml) and ethyl acetate (100 ml) were added. The mixture was neutralised with sodium hydrogen carbonate solution, the organic phase was collected. The aqueous phase was extracted with ethyl acetate (2×100 ml). The combined organic extracts were dried over magnesium sulphate, filtered and concentrated under reduced pressure to give the crude product. This material was recrystallised from hexane-15% ethyl acetate to give the clean product.

後処理

  1. stirringstirred at this temperature for 45 minutes
  2. temperatureto cool
  3. customthe organic phase was collected
  4. extractionThe aqueous phase was extracted with ethyl acetate (2×100 ml)
  5. dry with materialThe combined organic extracts were dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2f4013b1393544018ba1b01619748807
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05480873

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート