1H-Cyclopenta[l]phenanthrene → 2,3-Dihydro-1H-cyclopenta[l]phenanthrene
反応式
[CH2:1]1[C:5]2[C:6]3[C:11]([C:12]4[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=4[C:4]=2[CH:3]=[CH:2]1)=[CH:10][CH:9]=[CH:8][CH:7]=3.[H][H]>[Pd].C1(C)C=CC=CC=1>[CH2:3]1[C:4]2[C:17]3[C:12]([C:11]4[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=4[C:5]=2[CH2:1][CH2:2]1)=[CH:13][CH:14]=[CH:15][CH:16]=3参加物
5
実験手順
A mixture of 2 g cyclopentaphenanthrene, 0.2 g 10% palladium on carbon and 50 mL toluene was stirred under hydrogen (69 kPa) until hydrogen uptake ceased, about 48 h. Catalyst was removed by filtration through diatomaceous earth and the filtrate evaporated. The crude product remaining weighed 1.97 g. It was further purified by recrystallization from heptane at −40° C. to give 1.8 g colorless plates. Spectroscopic and chemical analysis confirmed the identity of the desired compound.
後処理
- customCatalyst was removed by filtration through diatomaceous earth
- customthe filtrate evaporated
- customIt was further purified by recrystallization from heptane at −40° C.
- customto give 1.8 g colorless plates
出典と根拠
- ORDレコード
- ord-19e147d26f284bde827d5b5af2a3eb28
- 出典データセット
- uspto-grants-2002_09
- 特許番号
- US06448358B2
反応ノート
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