Reaktion #824285

ord-d496930bdc2143efb06afa27cc8a3d3c

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution
  2. 2
    workup.ADDITIONcould be added to the resulting residue
  3. 3
    Waschenthe mixture could be washed with diethyl ether
  4. 4
    workup.ADDITIONThe aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution
  5. 5
    Extraktionextracted with methylene chloride
  6. 6
    WaschenThe organic layer could be washed with brine
  7. 7
    Trocknendried over sodium sulfate
  8. 8
    FiltrationAfter filtering
  9. 9
    Sonstigethe material could be purified by column chromatography

Vorschrift

The above compound could be made in the following manner: 1 eq. 2-Benzyl-morpholine-4-carboxylic acid tert-butyl ester could be dissolved in 4N solution of hydrogen chloride in dioxane and the mixture could be stirred at 60° C. for 3 h. The solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution could be added to the resulting residue, and the mixture could be washed with diethyl ether. The aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution and extracted with methylene chloride. The organic layer could be washed with brine and dried over sodium sulfate. After filtering, the material could be purified by column chromatography.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07595397B2uspto-grants-2009_09