반응 #74972

ord-eadd6e6b094b4f2faba7702ebf8734e5

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added slowly to a solution of 200 ml
  2. 2
    온도The solution was then cooled to 10°-13° C.
  3. 3
    기타a white precipitate formed
  4. 4
    여과This solid was filtered
  5. 5
    기타recrystallized from ethanol, m.p. 180°-181° C.

실험 절차

38 g. of 1,2,3,4,9,9-hexachloro-1,4,4a,8a-tetrahydro-1,4-methanonaphthalene-5,8-dione, prepared according to Example 1, were added slowly to a solution of 200 ml. of ethanol containing 20 ml. of 30% hydrogen peroxide and 13 g. of sodium carbonate at such a rate that the temperature was maintained at 40°-50° C. The yellow color of the dione disappeared quickly. The solution was then cooled to 10°-13° C. and a white precipitate formed. This solid was filtered and recrystallized from ethanol, m.p. 180°-181° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04174457uspto-grants-1979_11