Reaktion #11409

ord-f2219ebfb64740f68d7e74bc0bbba3d4

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated
  2. 2
    Sonstigeto remove THF
  3. 3
    WaschenThe aqueous phase was washed with ethyl ether
  4. 4
    ExtraktionThe acidified solution was extracted with Et2O or EtOAc (3X)
  5. 5
    Trocknendried over MgSO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated in vacuo
  8. 8
    Sonstigeto give a white solid

Vorschrift

To a solution of the ester of Example 6 in THF (0.8 mL) was added a solution of KOH (14 mg, 0.255 mmol) in H2O (0.2 mL). The mixture was stirred at 50° C., then concentrated to remove THF. The aqueous phase was washed with ethyl ether, then the aqueous phase was acidified until pH 3–4 was reached. The acidified solution was extracted with Et2O or EtOAc (3X), dried over MgSO4, filtered and concentrated in vacuo to give a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098223B2uspto-grants-2006_08