反応 #74973

ord-fecf5acb425f438aacae497ae513d550

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added 20 ml
  2. 2
    温度This reaction mixture was then heated at 130°-140° C. for 3 hours
  3. 3
    洗浄This solid was washed with Skelly "B" solvent several times on a Buchner funnel
  4. 4
    その他recrystallized from a Skelly "B"-benzene mixed solvent (20/80)
  5. 5
    その他Pale yellow crystals were obtained

実験手順

To a mixture of methyl-p-benzoquinone (60 g.), and hexachlorocyclopentadiene (140 g.), was added 20 ml. of toluene. This reaction mixture was then heated at 130°-140° C. for 3 hours. Upon cooling to room temperature the mixture solidified. This solid was washed with Skelly "B" solvent several times on a Buchner funnel and recrystallized from a Skelly "B"-benzene mixed solvent (20/80). Pale yellow crystals were obtained, m.p. 163°-165° C.

出典

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