Reaktion #499372

ord-32bdc9155d8b4068b02b321d3eb3b0f7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction was heated
  2. 2
    Temperaturat reflux overnight
  3. 3
    Extraktionextracted with 3× EtOAc
  4. 4
    TrocknenThe combined organic extracts were dried over Na2SO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo
  7. 7
    Sonstigeto give a solid, which
  8. 8
    Sonstigewas triturated with dichloromethane

Vorschrift

To a solution of the the product from Step F (802 mg, 2.23 mmol) in 50 mL of THF was added 10 mL of 2N NaOH solution, and the reaction was heated at reflux overnight. The solution was acidified with 1N HCl and extracted with 3× EtOAc. The combined organic extracts were dried over Na2SO4, filtered, and concentrated in vacuo to give a solid, which was triturated with dichloromethane to give the titled product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06562823B1uspto-grants-2003_05