Reaktion #67962

ord-1a20acba42b44c2fb88c7da546c2a2e8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe solvent was removed under reduced pressure
  2. 2
    SonstigeThe residue thus obtained
  3. 3
    SonstigeThe aqueous layer was separated
  4. 4
    workup.ADDITIONethyl acetate was added
  5. 5
    SonstigeThe organic layer was separated
  6. 6
    Trocknendried over potassium carbonate
  7. 7
    Sonstigethe solvent was removed under reduced pressure

Vorschrift

To 0.60 g of 1-tert-butyl 3-ethyl 4-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-1,3-dicarboxylate, 12 mL of 10 mol/L hydrogen chloride/ethanol was added, and the mixture was stirred for 2 hours, and then the solvent was removed under reduced pressure. The residue thus obtained was added with water and ethyl acetate. The aqueous layer was separated, ethyl acetate was added thereto, and the resultant solution was adjusted to pH 14 with a 5 mol/L aqueous sodium hydroxide solution. The organic layer was separated and dried over potassium carbonate, and the solvent was removed under reduced pressure to obtain 0.34 g of a brown oily substance, ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-2-carboxylate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524738B2uspto-grants-2013_09