Reaktion #74971

ord-ab4b133ffc3e4098bd2f1bbe49c66dce

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONwere dissolved in 60 ml
  2. 2
    SonstigeWhen the benzene was evaporated a white solid
  3. 3
    Sonstigewas obtained
  4. 4
    SonstigeOne recrystallization from benzene-Skelly B mixture
  5. 5
    Sonstigeyielded white crystals, m.p. 97°-98° C

Vorschrift

20 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 60 ml. of benzene and then 10 g. of n-butylmercaptan and a few crystals of ferric chloride were added. This reaction mixture was shaken for 24 hours (Parr shaker). When the benzene was evaporated a white solid was obtained. One recrystallization from benzene-Skelly B mixture yielded white crystals, m.p. 97°-98° C. The infrared spectrum showed strong carbonyl at 1750 cm-1.

Quelle

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