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

HRID 1907440Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1907440
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

Komponenten

3

Edukt 2

HCID 531671-MethylpiperazineHCID 679654-Fluoro-2-nitrotoluene

Produkt 1

HCID 581716321-Methyl-4-(4-methyl-3-nitrophenyl)piperazineAusbeute 48,3 %

Reaktionsbedingungen

Temperatur
200 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-a93557995aac4e9bacc2228476afc19f
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08598172B2

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