Reaktion #66577

ord-986826fa224b44c498e4e63b28714e72

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe mixture stirred at room temp for 16 h
  2. 2
    SonstigeThe reaction was quenched with methanol
  3. 3
    workup.ADDITIONdiluted with water
  4. 4
    Extraktionextracted with EtOAC
  5. 5
    EinengenThe organic extracts were concentrated in vacuo
  6. 6
    Sonstigethe residue was purified by chromatography (silica, 20% ether/hexane as eluent)

Vorschrift

Sodium hydride (88 mg, 60% wt.) was added portionwise to a solution of 4-BOC-piperazinone (400 mg) in DMF (10 ml). The reaction mixture was stirred for 1 h, and then benzyl bromide (262 μl) was added dropwise and the mixture stirred at room temp for 16 h. The reaction was quenched with methanol and diluted with water, and then extracted with EtOAC. The organic extracts were concentrated in vacuo and the residue was purified by chromatography (silica, 20% ether/hexane as eluent) to give the sub-title compound (429 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524715B2uspto-grants-2013_09