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1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one → 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one

HRID 2092578
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반응식

HRID 2092578 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[N:11]1[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1>COC(OC)N(C)C>[CH3:3][N:11]([CH:16]=[C:13]1[C:14](=[O:17])[CH2:15][CH2:16][N:11]([C:3]2[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=2[CH3:1])[CH2:12]1)[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 666567781-(2-Methyl-5-nitro-phenyl)-piperidin-4-one

생성물 1

HCID 673288983-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one

시약·촉매·용매 1

HCID 78373Dimethylformamide dimethyl acetal용매

실험 절차

A solution of 1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one [100 mg, 0.426 mmol] in N,N-Dimethylformamide dimethyl acetal (DMA.DMF) [1 ml] was heated to reflux for 12 hrs. After cooling to room temperature, reaction mixture was concentrated under vacuum. The dark brown crude product obtained was further purified by silica gel chromatography using 30-60% ethyl acetate/hexane as eluent to obtain pure desired product i.e., 3-Dimethylaminomethylene-1-(2-methyl-5-nitro-phenyl)-piperidin-4-one [4] as orange solid [Yield: 76.2 mg, 62.02%]

후처리

  • temperatureto reflux for 12 hrs
  • customreaction mixture
  • concentrationwas concentrated under vacuum
  • customThe dark brown crude product obtained
  • customwas further purified by silica gel chromatography
  • 출처 및 근거

    ORD 기록
    ord-243105bf2a244b4bbe5c981545d297bf
    출처 데이터셋
    uspto-grants-2013_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08440679B2

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