반응 #74971
ord-ab4b133ffc3e4098bd2f1bbe49c66dce
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.DISSOLUTIONwere dissolved in 60 ml
- 2기타When the benzene was evaporated a white solid
- 3기타was obtained
- 4기타One recrystallization from benzene-Skelly B mixture
- 5기타yielded white crystals, m.p. 97°-98° C
실험 절차
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.