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

HRID 1907440노트

반응식

HRID 1907440 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. until HPLC revealed the disappearance of the starting material. 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-a93557995aac4e9bacc2228476afc19f
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598172B2

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