1-Methylpiperazine → 2-Chloro-3-(4-methylpiperazin-1-YL)pyrazine

HRID 991663Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 991663
Cl[C:2]1[C:7]([Cl:8])=[N:6][CH:5]=[CH:4][N:3]=1.[CH3:9][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C(#N)C>[Cl:8][C:7]1[C:2]([N:13]2[CH2:14][CH2:15][N:10]([CH3:9])[CH2:11][CH2:12]2)=[N:3][CH:4]=[CH:5][N:6]=1

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 785752,3-Dichloropyrazine

Produkt 1

HCID 220363522-Chloro-3-(4-methylpiperazin-1-YL)pyrazineAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 2,3-dichloropyrazine (10.1 g, 68 mmol) and N-methylpiperazine (10.15 g, 100 mmol) in acetonitrile (250 mL) was stirred at room temperature for 60 h. The solvent was removed under reduced pressure and the residue was taken up in CHCl3/brine. The dried (MgSO4) organic layer was concentrated and the remaining oil was purified by chromatography on silica gel using CHCl3/MeOH (95:5) as eluent to give 10.7 g (75%) of the title compound as an oil that crystallized upon standing: mp 34-36° C. Anal. (C9H13ClN4) C, H, N.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. dry with materialThe dried (MgSO4) organic layer
  3. concentrationwas concentrated
  4. customthe remaining oil was purified by chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-f543c41e355f43cd9a16c7631bbd89cc
Quelldatensatz
uspto-grants-2002_10
Patentnummer
US06465467B1

Notizen zur Reaktion

Wird geladen…