Reaktion #1671975

ord-efa5215072614c969ea39bdbeb430386

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was heated
  2. 2
    Temperaturto reflux
  3. 3
    Temperaturcooled
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    Waschenthe organic phase washed with 8% sodium bicarbonate solution (3×20 ml)
  6. 6
    Sonstigedried
  7. 7
    Einengenconcentrated in vacuo
  8. 8
    SonstigeThe crude material was purified by FCC
  9. 9
    Wascheneluted with dichloromethane-hexane (1:1) to dichloromethane-hexane (2:1)

Vorschrift

7-([1,3]-Dioxan-2-yl)-5-(5-trifluoromethyl-tetrazol-1-yl)-benzofuran (160 mg) was dissolved in tetrahydrofuran (30 ml) and dilute hydrochloric acid (20 ml; 2M). The reaction mixture was heated to reflux and stirred for a total of 3 h, cooled and concentrated in vacuo. The residue was taken up in chloroform (40 ml), and the organic phase washed with 8% sodium bicarbonate solution (3×20 ml), dried and concentrated in vacuo. The crude material was purified by FCC eluted with dichloromethane-hexane (1:1) to dichloromethane-hexane (2:1) to give the title compound (100 mg) as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05935972uspto-grants-1999_08