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Dimethylformamide → HCID 9795416, 화합물

HRID 1249757
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인쇄 미리보기

반응식

HRID 1249757 반응식
[H-].[Na+].[CH2:3]=[C:4]1[C:16]2[NH:15][C:14]3[C:9](=[CH:10][C:11]([O:17][CH3:18])=[CH:12][CH:13]=3)[C:8]=2[CH2:7][CH2:6][N:5]1[C:19](=[O:21])[CH3:20].CN(C=[O:26])C>>[C:19]([N:5]1[CH2:6][C:7]2[C:8](=[O:26])[C:9]3[CH:10]=[C:11]([O:17][CH3:18])[CH:12]=[CH:13][C:14]=3[NH:15][C:16]=2[C:4]1=[CH2:3])(=[O:21])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 15816962HCID 15816962, 화합물

생성물 1

HCID 9795416HCID 9795416, 화합물

실험 절차

NaH (1.5 eq; 60% suspension in oil) is added to a solution of 1-methylene-2-acetyl-6-methoxy-1,2,3,4-tetrahydro-β-carboline (1 g; 3.9 mmol) in DMF (5 ml). The mixture is stirred under an oxygen atmosphere overnight. The DMF is then distilled off under reduced pressure. The crude product is washed successively with ethyl acetate, methanol and then ether. After drying, 2-acetyl-7-methoxy-3-methylene-9-oxo-1,3,4,9-tetrahydropyrrolo[3,4-b]quinoline is obtained.

후처리

  1. distillationThe DMF is then distilled off under reduced pressure
  2. washThe crude product is washed successively with ethyl acetate, methanol
  • customAfter drying
  • 출처 및 근거

    ORD 기록
    ord-624b042d7cc948eebccd83d54b449b2c
    출처 데이터셋
    uspto-grants-2002_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06335346B1

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