Hydrochloric Acid → 1-(3-fluoro-4-methoxyphenyl)propan-2-one
反応式
Cl.[F:2][C:3]1[CH:4]=[C:5]([CH:11]=[C:12]([N+]([O-])=O)[CH3:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[O:17]1CCCC1>[Fe]>[F:2][C:3]1[CH:4]=[C:5]([CH2:11][C:12](=[O:17])[CH3:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]参加物
5
実験手順
Concentrated hydrochloric acid (30 ml) was added dropwise, over 45 minutes, to a stirred mixture of iron powder (6 g) and 1-(3-fluoro-4-methoxyphenyl)-2-nitroprop-1-ene (5.7 g) in tetrahydrofuran (100 ml) at reflux. The mixture was heated under reflux for a further two hours, cooled, filtered and evaporated. Water (100 ml) was added to the residue and extracted with dichloromethane. The dried (magnesium sulphate) extracts were evaporated to dryness to give the title compound as an oil.
後処理
- temperatureat reflux
- temperatureThe mixture was heated
- temperatureunder reflux for a further two hours
- temperaturecooled
- filtrationfiltered
- customevaporated
- additionWater (100 ml) was added to the residue
- extractionextracted with dichloromethane
- dry with materialThe dried (magnesium sulphate) extracts
- customwere evaporated to dryness
出典と根拠
- ORDレコード
- ord-4f24f1be4ad34e689f1f0714fbfa20f4
- 出典データセット
- uspto-grants-1986_11
- 特許番号
- US04622342
反応ノート
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