2-Bromo-1-chloro-4-(trifluoromethoxy)benzene → 1-Chloro-2-vinyl-4-(trifluoromethoxy)benzene
反応式
Br[C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[CH:4][C:3]=1[Cl:13].[CH2:14](C([Sn])=C(CCCC)CCCC)[CH2:15]CC>C1(C)C=CC=CC=1>[Cl:13][C:3]1[CH:4]=[CH:5][C:6]([O:8][C:9]([F:12])([F:11])[F:10])=[CH:7][C:2]=1[CH:14]=[CH2:15]参加物
4
実験手順
2-Bromo-1-chloro-4-(trifluoromethoxy)benzene (Description 25; 1.0 g, 3.6 mmol) and tri-n-butylvinyl tin (1.21 g, 3.8 mmol) were dissolved in toluene (20 mL) and the solution was degassed for 45 minutes with nitrogen. Tetrakis(triphenylphosphine) palladium (0) (100 mg) was then added and the solution heated at reflux for 2 hours. Once cooled, the solution was concentrated and the residue was purified by silica chromatography to give the title compound (274 mg, 1.2 mmol).
後処理
- customthe solution was degassed for 45 minutes with nitrogen
- additionTetrakis(triphenylphosphine) palladium (0) (100 mg) was then added
- temperaturethe solution heated
- temperatureat reflux for 2 hours
- temperatureOnce cooled
- concentrationthe solution was concentrated
- customthe residue was purified by silica chromatography
出典と根拠
- ORDレコード
- ord-42516b6a83aa443da1d965425cf9656c
- 出典データセット
- uspto-grants-2003_04
- 特許番号
- US06555552B2
反応ノート
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