Reaktion #43139

ord-6c9988accec348ea9bff4032ff9d99e2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture heated
  2. 2
    Temperaturto reflux for 2 hours
  3. 3
    SonstigeThe Solvent was removed by rotary evaporation
  4. 4
    Sonstigethe solvent again removed
  5. 5
    Sonstigeto remove residual water

Vorschrift

Intermediate 82 was dissolved in 200 mL of 48% aqueous HBr and the mixture heated to reflux for 2 hours. The Solvent was removed by rotary evaporation. The residue was taken up in 100 mL of ethanol and the solvent again removed. This was repeated twice more to remove residual water. LC-MS showed the product was >90% pure had the expected M+H+ of 156.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732444B2uspto-grants-2010_06