反応式
[CH:1]1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=C[CH:2]=1.Br[C:21]1[CH:26]=[C:25]([N+:27]([O-:29])=[O:28])[C:24]([F:30])=[CH:23][C:22]=1[F:31].C([Sn](CCCC)(CCCC)C=C)CCC.[F-].[Na+]>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(OCC)C>[F:30][C:24]1[CH:23]=[C:22]([F:31])[C:21]([CH:1]=[CH2:2])=[CH:26][C:25]=1[N+:27]([O-:29])=[O:28]参加物
8
実験手順
A mixture of Pd2 dba3 (1.924 g, 2.101 mmol), and PPh3 (2.204 g, 8.404 mmol) was dissolved in toluene (200 mL), degassed and then stirred 10 minutes at ambient temperature. A solution of 1-bromo-2,4-difluoro-5-nitrobenzene (10 g, 42.02 mmol) in toluene (200 mL) was then added to the above solution, followed by tributyl(vinyl)stannane (18.40 mL, 63.03 mmol). The mixture was refluxed for 2 hours, then poured into a mixture of aqueous NaF and diethyl ether. The residue was purified using silica gel column chromatography with 5-10-20% acetone in hexanes to provide 1,5-difluoro-2-nitro-4-vinylbenzene (6 g, 32.41 mmol, 77.13% yield) as yellow oil.
後処理
- customdegassed
- temperatureThe mixture was refluxed for 2 hours
- customThe residue was purified
出典と根拠
- ORDレコード
- ord-c0a0e835fffe4cffbb63f0065405a988
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08754226B2
関連ノート
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