Reaktion #8276

ord-5ffcee3aef244c46ad73a59445cc6d99

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigemethanol evaporated
  2. 2
    ExtraktionThe residual aqueous solution was extracted with dichloromethane (2×20 ml)
  3. 3
    Waschenthe extracts washed with brine (20 ml)
  4. 4
    Sonstigeevaporated
  5. 5
    SonstigeThe resulting solid was triturated with isohexane (50 ml)

Vorschrift

Di-(t-butoxycarbonyl)aminopyrazine (2.1 g, 7.1 mM) in methanol (50 ml) under nitrogen, was treated with aqueous sodium hydroxide (2.5 M, 2.84 ml, 7.1 mM), and stirred at ambient temperature for 2 hours. The mixture was neutralised by the addition of water (25 ml) and solid carbon dioxide, then methanol evaporated. The residual aqueous solution was extracted with dichloromethane (2×20 ml), the extracts washed with brine (20 ml) and evaporated. The resulting solid was triturated with isohexane (50 ml) to give the title product as a white solid (1.03 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087629B2uspto-grants-2006_08