反応式
[F:1][C:2]1[CH:3]=[C:4]([C:17]2[CH:26]=[CH:25][C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=2)[CH:5]=[CH:6][C:7]=1[CH:8]=[CH:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=1>[Pd].C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]([C:17]2[CH:26]=[CH:25][C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=2)[CH:5]=[CH:6][C:7]=1[CH2:8][CH2:9][C:10]1[CH:11]=[CH:12][C:13]([F:16])=[CH:14][CH:15]=1参加物
実験手順
A 30 ml Solumix/toluene (1:1) solution of 3.44 g (=10.05 mmol) of the above 2-{3-fluoro-4-[2-(4-fluorophenyl)vinyl]phenyl}naphthalene was added with 0.17 g of 5%-Pd/C and then stirred for 20 hours in an H2-atmosphere. The 5%-Pd/C was filtrated away from the reaction solution, and the filtrate was condensed under a reduced pressure. The obtained gray solid of 3.66 g was purified with silica gel chromatography using toluene as the eluent to obtain a white solid of 3.29 g, which was further recrystallized with a mixed solvent of heptane/toluene in a ratio of 5:4 to obtain a product of 3.15 g. The product was characterized as the target compound based on results of various instrumental analyses, and the phase transition of the product is notated as “C 154.3 I”.
後処理
- filtrationThe 5%-Pd/C was filtrated away from the reaction solution
- customcondensed under a reduced pressure
- customThe obtained gray solid of 3.66 g was purified with silica gel chromatography
- customto obtain a white solid of 3.29 g, which
- customwas further recrystallized with a mixed solvent of heptane/toluene in a ratio of 5:4
- customto obtain a product of 3.15 g
- customon results of various instrumental analyses
出典と根拠
- ORDレコード
- ord-65f89ede07124d00b9d1f1e2aab10b5c
- 出典データセット
- uspto-grants-2010_09
- 特許番号
- US07790915B2
関連ノート
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