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1,2-Dimethylindole → 1-(1,2-dimethyl-1H-indol-3-yl)ethanone

HRID 1708602
ノート
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反応式

HRID 1708602 の反応式
CN(C)[C:3](=[O:5])[CH3:4].P(Cl)(Cl)(Cl)=O.[CH3:12][N:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[C:14]1[CH3:22]>>[C:3]([C:15]1[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:13]([CH3:12])[C:14]=1[CH3:22])(=[O:5])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 134081,2-DimethylindoleHCID 24813Phosphorus oxychlorideHCID 31374Dimethylacetamide

生成物 1

HCID 2857551-(1,2-dimethyl-1H-indol-3-yl)ethanone収率 80%

実験手順

To a solution of 6 moles of N,N-dimethylacetamide and cooled at 0° C., 1.5 moles of phosphorus oxychloride was added dropwise in 30 minutes with stirring. After further adding 1 mole of 1,2-dimethylindole thereto, the reaction was carried out at 85°-90° C. for 2 hours. Then, the reaction solution was poured into 2 liters of ice water. The reaction solution was made alkaline, extracted with 0.5 liter of ethyl acetate, washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue was recrystallized from ethyl acetate to give yellow crystals in yield of 80%.

後処理

  1. extractionextracted with 0.5 liter of ethyl acetate
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was recrystallized from ethyl acetate
  6. customto give yellow crystals in yield of 80%

出典と根拠

ORDレコード
ord-ead1894bfcef416dbf89e976647c406a
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05359085

反応ノート

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