반응식
[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]=1참가 물질
실험 절차
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”.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-65f89ede07124d00b9d1f1e2aab10b5c
- 출처 데이터셋
- uspto-grants-2010_09
- 특허 번호
- US07790915B2
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