Reaktion #42093

ord-6580fa0bfeac4e7fad3eaafdcf660b82

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenbefore concentrating
  2. 2
    workup.DISSOLUTIONThe product was dissolved in EtOAc
  3. 3
    Waschenwashed with saturated aqueous NaHCO3 solution
  4. 4
    EinengenThe solution was concentrated
  5. 5
    Sonstigepurified via flash chromatography on silica gel with a gradient elution of 0% to 20% EtOAc in hexane affording the title compound

Vorschrift

To the product of Step C (300 mg) was added H2NCH3 (3.34 mL, 2 M solution in THF). The reaction stirred at room temperature overnight before concentrating. The product was dissolved in EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0% to 20% EtOAc in hexane affording the title compound. HPLC/MS: 353.9 (M+1), 355.9 (M+3); Rt=4.21 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728141B2uspto-grants-2010_06