Piperazine → 1-(3-Fluoro-1-oxido-2-pyridinyl)piperazine

HRID 1263223Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1263223
Cl[C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:9].[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C(O)CCC>[N:10]1([C:2]2[C:7]([F:8])=[CH:6][CH:5]=[CH:4][N+:3]=2[O-:9])[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

Komponenten

4

Edukt 2

HCID 4837PiperazineHCID 49131402-Chloro-3-fluoropyridine N-oxide

Produkt 1

HCID 704816081-(3-Fluoro-1-oxido-2-pyridinyl)piperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

A solution of 2-chloro-3-fluoropyridine N-oxide (400 mg, 3.0 mmol) and piperazine (1.3 g, 15 mmol) in n-butanol, 15 ml, is stirred at reflux for 20 hours. After concentrating under reduced pressure at 55°-60° C., the residue is chromatographed over silica gel and the crude N-oxide eluted with a 50% methanol-methylene chloride solvent mixture. The appropriate eluate is concentrated to an oily residue of the title compound.

Aufarbeitung

  1. temperatureat reflux for 20 hours
  2. concentrationAfter concentrating under reduced pressure at 55°-60° C.
  3. customthe residue is chromatographed over silica gel
  4. washthe crude N-oxide eluted with a 50% methanol-methylene chloride solvent mixture
  5. concentrationThe appropriate eluate is concentrated to an oily residue of the title compound

Quellen und Nachweise

ORD-Eintrag
ord-6a3fe72decea4c029480d68a3e741bac
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04456604

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