Reaktion #159072

ord-4284c186bf324ba394c57f61081eb85c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe organic solvents were removed in vacuo
  2. 2
    workup.ADDITIONThe crude mixture was diluted with water and EtOAc
  3. 3
    Sonstigethe organic layer was collected
  4. 4
    SonstigeAll volatiles were removed in vacuo
  5. 5
    Sonstigethe crude acid was used without further purification

Vorschrift

5-Aza-spiro[2.4]heptane-5,6-dicarboxylic acid 5-benzyl ester 6-methyl ester (244 mg, 0.840 mmol) was dissolved in THF (2.0 mL)/MeOH (1.5 mL). An aqueous solution of LiOH (35.5 mg, 0.84 mmol) was added and stirring at room temperature was continued. After 3 hours, the reaction was neutralized with aqueous HCl (1M) and the organic solvents were removed in vacuo. The crude mixture was diluted with water and EtOAc and the organic layer was collected. All volatiles were removed in vacuo and the crude acid was used without further purification. LCMS-ESI+: calc'd for C15H17NO4: 275.3 (M+). Found: 276.3 (M+H+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822430B2uspto-grants-2014_09