Reaktion #2349692

ord-ea3aa07249104d4b9ae9a0a7e629e8ca

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed in vacuo
  2. 2
    ExtraktionThe aqueous phase was extracted with DCM (2×10 mL)
  3. 3
    TrocknenThe combined organic layers were dried (MgSO4)
  4. 4
    Sonstigethe solvent removed in vacuo

Vorschrift

To 3-[4-(2,4-difluoro-phenyl)-piperazine-1-carbonyloxymethyl]-morpholine-4-carboxylic acid tert-butyl ester (170 mg, 0.39 mmol) in DCM (5 mL) at 0° C. was added TFA (1 mL in 5 mL DCM). The reaction mixture was allowed to warm to room temperature and stirred overnight. The solvent was removed in vacuo and the residue suspended between sat aq NaHCO3 (10 mL) and DCM (10 mL). The aqueous phase was extracted with DCM (2×10 mL). The combined organic layers were dried (MgSO4) and the solvent removed in vacuo to give morpholin-3-ylmethyl 4-(2,4-difluorophenyl)piperazine-1-carboxylate (104 mg, 79%) as a colourless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07851471B2uspto-grants-2010_12