反応 #74970

ord-913d1322b7d14de4aa470eee16f6e226

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONwere dissolved in 250 ml
  2. 2
    温度This reaction mixture was heated at 40°-45° C. for 12 hours
  3. 3
    その他the benzene was evaporated
  4. 4
    その他The white solid residue obtained
  5. 5
    その他was recrystallized from benzene twice
  6. 6
    その他yielded white crystals, m.p. 157°-158° C

実験手順

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%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04174457uspto-grants-1979_11