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

HRID 1914753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1914753
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

Komponenten

3

Edukt 2

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

Produkt 1

HCID 594543161-[2-(4-Methyl-1-piperazinyl)-6-nitrophenyl]ethanoneAusbeute 68,9 %

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

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.

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 crude was purified by flash chromatography (acetone/MeOH 75:25)

Quellen und Nachweise

ORD-Eintrag
ord-5aa2c5b36fc14360af46dff00959ba66
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08614220B2

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