Reaktion #217117

ord-d908b1a781a24b548584b88d653c6563

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture is filtered over kieselgur with suction
  2. 2
    Waschenwashed with 300 ml of methylene chloride
  3. 3
    EinengenThe methylene chloride phase is concentrated in vacuo
  4. 4
    Sonstigethe residue is chromatographed on a column (150 g of silica gel 70-230 mesh, φ3.5 cm, using ethyl acetate/petroleum ether 2:8)

Vorschrift

10.3 g (48 mmol) of pyridinium chlorochromate and 4.9 (48 mmol) of neutral alumina are added to a solution of 3.8 g (12 mmol) of the compound from Example 4 in 100 ml of methylene chloride p.a. and the mixture is stirred for 1 h at room temperature. The mixture is filtered over kieselgur with suction and washed with 300 ml of methylene chloride. The methylene chloride phase is concentrated in vacuo and the residue is chromatographed on a column (150 g of silica gel 70-230 mesh, φ3.5 cm, using ethyl acetate/petroleum ether 2:8).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05470982uspto-grants-1995_11