Potassium Carbonate → HCID 22326840, Verbindung

HRID 495463Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 495463
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[O:14][CH3:15].[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C([O-])([O-])=O.[K+].[K+]>CC#N>[CH3:15][O:14][C:6]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=1[O:4][CH2:3][CH2:2][N:20]1[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 22326897HCID 22326897, Verbindung

Produkt 1

HCID 22326840HCID 22326840, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 1-(2-chloroethoxy)-2-methoxy-4-nitrobenzene (Step A, 1 eq), N-methylpiperazine (3 eq) and K2CO3 (2.5 eq) in CH3CN was stirred and heated under reflux until HPLC indicated the reaction was complete. The resulting solid was filtered, rinsed well with CH2Cl2 and the filtrate and washings were combined, concentrated and purified by column chromatography giving 1-[2-(2-methoxy-4-nitro-phenoxy)-ethyl]-4-methyl-piperazine.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux until HPLC
  3. filtrationThe resulting solid was filtered
  4. washrinsed well with CH2Cl2
  5. concentrationconcentrated
  6. custompurified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-7751c82824fa4fd3a6a4caa84299b606
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06939874B2

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