Reaktion #215258

ord-eba45b1c03934e9d9e0cf449e29a48ff

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONis dissolved in 150 ml
  2. 2
    Filtrationthe solution is filtered
  3. 3
    Sonstigeto remove insoluble materials
  4. 4
    Temperaturcooled
  5. 5
    Sonstigeyielding orange crystals, which
  6. 6
    Filtrationare filtered
  7. 7
    Waschenwashed with glacial acetic acid
  8. 8
    Sonstigedried

Vorschrift

A mixture of isomers of 1,4-dimethoxy-11,12-dihydroxy-9,10-ethano-anthracene weighing 10 g. is dissolved in 150 ml. of glacial acetic acid at 50° C. and treated portionwise with 30 g. of lead tetraacetate. After 2 hours at 50° C., the solution is filtered to remove insoluble materials and cooled yielding orange crystals, which are filtered, washed with glacial acetic acid and dried, m.p. 208°-212° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04258181uspto-grants-1981_03