Reaktion #8913

ord-e1aac933471c4119887b78fda5452eab

Lösungsmittel

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenAfter 3 h the reaction was concentrated
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in dichloromethane
  3. 3
    Waschenwashed twice with aqueous sodium bicarbonate
  4. 4
    EinengenThe solution was then concentrated
  5. 5
    Sonstigethe residue was purified via flash chromatography on silica gel with gradient elution of 0–60% ethyl acetate in hexanes affording the title compound

Vorschrift

The product of Example 100 (0.200 g), acetic anhydride (1.25 mL) and acetic acid (0.25 mL) were combined and then heated to 85° C. After 3 h the reaction was concentrated and the residue was dissolved in dichloromethane and washed twice with aqueous sodium bicarbonate. The solution was then concentrated and the residue was purified via flash chromatography on silica gel with gradient elution of 0–60% ethyl acetate in hexanes affording the title compound. HPLC/MS: 483.0 (M+1), 484.8 (M+3); Rt=3.95-min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091216B2uspto-grants-2006_08