1-Methylpiperazine → 1-Methyl-4-(4-methyl-3-nitrophenyl)piperazine

HRID 1914755노트

반응식

HRID 1914755 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[CH3:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>>[CH3:12][N:13]1[CH2:18][CH2:17][N:16]([C:2]2[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=2)[CH2:15][CH2:14]1

참가 물질

3

반응물 2

HCID 531671-MethylpiperazineHCID 679654-Fluoro-2-nitrotoluene

생성물 1

HCID 581716321-Methyl-4-(4-methyl-3-nitrophenyl)piperazine수율 48.3%

반응 조건

온도
200 °C

실험 절차

In a cylindrical quartz tube were placed 4-fluoro-1-methyl-2-nitro-benzene (20.0 g, 129 mmol) and N-methyl-piperazine (26 g, 258 mmol). The reaction was heated for 48 hours at 200° 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 and the solvent was removed under reduced pressure. The final compound (14.65 g, 48% yield) was obtained as a brown oil.

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 solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-64851bc0958c4764b9104c2e5d93f5ee
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614220B2

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