1-Methylpiperazine → 1-[2-(4-Methyl-1-piperazinyl)-6-nitrophenyl]ethanone

HRID 1914753노트

반응식

HRID 1914753 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=1[C:11](=[O:13])[CH3:12].[CH3:14][N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1>>[CH3:14][N:15]1[CH2:20][CH2:19][N:18]([C:2]2[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=2[C:11](=[O:13])[CH3:12])[CH2:17][CH2:16]1

참가 물질

3

반응물 2

HCID 531671-MethylpiperazineHCID 204565701-(2-Chloro-6-nitrophenyl)ethan-1-one

생성물 1

HCID 594543161-[2-(4-Methyl-1-piperazinyl)-6-nitrophenyl]ethanone수율 68.9%

반응 조건

온도
120 °C

실험 절차

In a cylindrical quartz tube were placed 1-(2-chloro-6-nitro-phenyl)-ethanone (300 mg, 1.5 mmol) and N-methyl-piperazine (12 ml, 180 mmol). The reaction was heated for 40 hours at 120° C. The solvent was removed under reduced pressure and the residue was dissolved in DCM. The solution was washed twice with water and the organic phase was dried over anhydrous Na2SO4. The crude was purified by flash chromatography (acetone/MeOH 75:25) affording the desired compound (272 mg, 46% yield), as a yellow solid.

후처리

  1. customIn a cylindrical quartz tube were placed
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in DCM
  4. washThe solution was washed twice with water
  5. dry with materialthe organic phase was dried over anhydrous Na2SO4
  6. customThe crude was purified by flash chromatography (acetone/MeOH 75:25)

출처 및 근거

ORD 기록
ord-5aa2c5b36fc14360af46dff00959ba66
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614220B2

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