Reaktion #157337

ord-4b1f7a728c924ed3b5a085862a391f3d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe reaction mixture was concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONdissolved in 1 N NaOH
  3. 3
    Extraktionextracted with EtOAc (3×)
  4. 4
    TrocknenThe combined extracts were dried over Na2SO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

4 M HCl in 1,4-dioxane (6 mL, 24 mmol) was added to a solution of tert-butyl 4-(benzo[d]thiazol-6-ylcarbamoyl)-3-((pyridin-3-yloxy)methyl)piperazine-1-carboxylate di-TFA salt (154 mg, 0.221 mmol) in MeOH (1 mL). After stirring overnight, the reaction mixture was concentrated under reduced pressure, dissolved in 1 N NaOH, and extracted with EtOAc (3×). The combined extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure, yielding 69.5 mg (85%) of the title compound as an off-white solid. LC-MS: RT=3.62 min, [M+H]+=370.1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822472B2uspto-grants-2014_09