Reaktion #1782269

ord-089f68b08fe543bfbdedd8c9521524ae

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeall volatiles are removed in vacuo
  2. 2
    SonstigeThe crude product is purified by flash column chromatography with dichloromethane/methanol (95:5 to 10:1)

Vorschrift

Azide 23 (Example 10, 100 mg, 0.23 mmol) is dissolved in 0.9 mL of 1,4-dioxane/H2O (8:1), and 0.3 mL of a trimethylphospine solution (1 M in THF) is added. The reaction is stirred at room temperature for 3 h, then all volatiles are removed in vacuo. The crude product is purified by flash column chromatography with dichloromethane/methanol (95:5 to 10:1). Yield: 87 mg (0.021 mmol, 91%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08163479B2uspto-grants-2012_04