Reaktion #217115

ord-d33d8e64620447a79867ab5180bdf7fe

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationIt is then filtered over kieselgur with suction
  2. 2
    Extraktionthe methylene chloride phase is extracted three times
  3. 3
    Trocknendried over magnesium sulphate
  4. 4
    EinengenAfter concentrating in vacuo
  5. 5
    Sonstigethe residue is chromatographed on a column (100 g of silica gel 70-230 mesh, φ3

Vorschrift

3.8 g (16.4 mmol) of 2,3-dichloro-5,6-dicyano-p-benzoquinone are added to a solution of 6.6 g (16.4 mmol) of the compound from Example 2 in 200 ml of methylene chloride p.a. and the mixture is stirred for 1 h at room temperature. It is then filtered over kieselgur with suction, the methylene chloride phase is extracted three times using 100 ml of water each time and dried over magnesium sulphate. After concentrating in vacuo, the residue is chromatographed on a column (100 g of silica gel 70-230 mesh, φ3.5 cm, using ethyl acetate/petroleum ether (1:9).

Quelle

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