Reaktion #89751

ord-8a028f4803844a06b97490d17c5d9695

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter quenched with water
  2. 2
    Extraktionthe mixture was extracted with ethyl acetate
  3. 3
    WaschenThe combine organic lyers were washed with brine
  4. 4
    Sonstigedried
  5. 5
    Einengenconcentrated
  6. 6
    Sonstigeto dry
  7. 7
    SonstigeThe residue was used directly in next step without further purification

Vorschrift

To a mixture of (2S,3S,5S)-5-methoxy-3-(methoxycarbonyl)piperidine-2-carboxylic acid (14.0 mg, 0.0000644 mol), 1-phenyl-piperazine (0.01231 mL, 8.056E-5 mol) and benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (35.63 mg, 8.056E-5 mol) in N,N-dimethylformamide (0.20 mL, 0.0026 mol) was added N,N-diisopropylethylamine (0.01403 mL, 8.056E-5 mol). The mixture was stirred at rt for 2 h. After quenched with water, the mixture was extracted with ethyl acetate. The combine organic lyers were washed with brine, dried and concentrated to dry. The residue was used directly in next step without further purification. MS (ESI): (M+H)+=362.1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440958B2uspto-grants-2016_09