Reaktion #74970

ord-913d1322b7d14de4aa470eee16f6e226

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONwere dissolved in 250 ml
  2. 2
    TemperaturThis reaction mixture was heated at 40°-45° C. for 12 hours
  3. 3
    Sonstigethe benzene was evaporated
  4. 4
    SonstigeThe white solid residue obtained
  5. 5
    Sonstigewas recrystallized from benzene twice
  6. 6
    Sonstigeyielded white crystals, m.p. 157°-158° C

Vorschrift

38 g. of 1,2,3,4,9,9-hexachloro-1,4,4a,8a-tetrahydro-1,4-methanonaphthalene-5,8-dione, prepared as in Example 1, were dissolved in 250 ml. of benzene, 15 g. of freshly generated benzene sulfinic acid were added and then a few drops of water were added. This reaction mixture was heated at 40°-45° C. for 12 hours and then the benzene was evaporated. The white solid residue obtained was recrystallized from benzene twice and yielded white crystals, m.p. 157°-158° C. The yield was about 88%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04174457uspto-grants-1979_11