Reaktion #672989

ord-9fba0551216d4bb9863990278e4a6d6a

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed
  2. 2
    Sonstigethe residue was partitioned between dichloromethane and brine
  3. 3
    Trocknendried with MgSO4
  4. 4
    Sonstigethe solvent was evaporated
  5. 5
    SonstigeChromatography on silica gel (dichloromethane/methanol 98:2) yielded the intermediate silyl-protected alcohol (124 mg, 76%), MS

Vorschrift

(10aR)-9-Bromo-1,2,3,4,10,10a-hexahydro-pyrazino[1,2-a]indole (0.10 g, 0.39 mmol) and 2-(bromoethoxy)-tert-butyl-dimethylsilane (88 mg, 0.39 mmol) were dissolved in acetonitrile (2 mL). Potassium carbonate (63 mg, 0.46 mmol) was added and the solution was boiled with stirring for 2 d. The solvent was removed and the residue was partitioned between dichloromethane and brine. The organic phases were pooled, dried with MgSO4 and the solvent was evaporated. Chromatography on silica gel (dichloromethane/methanol 98:2) yielded the intermediate silyl-protected alcohol (124 mg, 76%), MS: m/e=413.3 (M+H+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06933387B2uspto-grants-2005_08