Reaktion #89752

ord-11bc39fb4e5d41da9dd49d4b36931e4f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter quenched with aq. sodium bicaronate
  2. 2
    Extraktionthe reaction was extracted with ethyl acetate
  3. 3
    WaschenThe combined organic layers were washed with brine
  4. 4
    Sonstigedried
  5. 5
    Einengenconcentrated
  6. 6
    Sonstigeto dry

Vorschrift

To a mixture of methyl(2S,3S,5S)-5-methoxy-2-[(4-phenylpiperazin-1-yl)carbonyl]piperidine-3-carboxylate (0.0233 g, 0.0000645 mol) and 4-dimethylaminopyridine (0.0118 g, 0.0000967 mol) in methylene chloride (1.00 mL, 0.0156 mol) was added methyl chloroformate (0.00648 mL, 0.0000838 mol). The reaction was stirred at rt overnight. After quenched with aq. sodium bicaronate, the reaction was extracted with ethyl acetate. The combined organic layers were washed with brine, dried, concentrated to dry. The resulting residue was used directly in next step. MS (ESI): (M+H)+=420.2.

Quelle

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