Reaktion #731366

ord-3633d7d9aee0424e811f60bf1970bb0a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe solution was concentrated in vacuo
  2. 2
    Sonstigethe residue was purified by RPHPLC
  3. 3
    Wascheneluting with a gradient of 20% through 60% acetonitrile in 0.05% aq HCl over 320 min
  4. 4
    workup.ADDITIONThe clean product containing fractions
  5. 5
    Einengenpartially concentrated

Vorschrift

2-[4-(tert-Butyl)-2-(1-Boc-piperidin-4-yloxy)benzoylamino]-N-(5-chloropyridin-2-yl)-4-chlorobenzamide (0.4 g, 0.64 mmol) was dissolved in 4 N HCl/p-dioxane (15 mL). After stirring for 30 min, the solution was concentrated in vacuo and the residue was purified by RPHPLC, eluting with a gradient of 20% through 60% acetonitrile in 0.05% aq HCl over 320 min. The clean product containing fractions were combined, partially concentrated and lypholyzed to give 0.0864 g (23%) of white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07700628B2uspto-grants-2010_04