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

HRID 1708602
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반응식

HRID 1708602 반응식
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]
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참가 물질

4

반응물 3

HCID 134081,2-DimethylindoleHCID 24813Phosphorus oxychlorideHCID 31374Dimethylacetamide

생성물 1

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

실험 절차

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%.

후처리

  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%

출처 및 근거

ORD 기록
ord-ead1894bfcef416dbf89e976647c406a
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05359085

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