(E)-N-[2-(6-methoxyindan-1-ylidene)ethyl]acetamide → N-[2-(5-Methoxy-1H-inden-3-yl)ethyl]acetamide

HRID 582210ノート

反応式

HRID 582210 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8]/[C:9]/2=[CH:12]\[CH2:13][NH:14][C:15](=[O:17])[CH3:16])=[CH:5][CH:4]=1>FC(F)(F)C(O)=O.O1CCCC1.O>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6](=[CH:5][CH:4]=1)[CH2:7][CH:8]=[C:9]2[CH2:12][CH2:13][NH:14][C:15](=[O:17])[CH3:16]

参加物

5

反応物 1

HCID 59957023(E)-N-[2-(6-methoxyindan-1-ylidene)ethyl]acetamide

生成物 1

HCID 54016815N-[2-(5-Methoxy-1H-inden-3-yl)ethyl]acetamide収率 90.1%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6422Trifluoroacetic acid溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

The (E)-N-[2-(6-methoxyindan-1-ylidene)ethyl]-acetamide (1.0 g, 4.32 mmol) thus obtained was dissolved in trifluoroacetic acid(6 ml)-tetrahydrofuran(6 ml) and the solution was refluxed for 1.5 hours. This reaction mixture was poured in water and extracted with ethyl acetate. The extract was washed serially with saturated saline and water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-methanol=96:4) to provide the title compound (yield 0.9 g, 90%).

後処理

  1. temperaturethe solution was refluxed for 1.5 hours
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed serially with saturated saline and water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate-methanol=96:4)

出典と根拠

ORDレコード
ord-4565cd77d32543e7903de635a35c357a
出典データセット
uspto-grants-1999_07
特許番号
US05922771

反応ノート

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