Hydrochloric Acid → 1-(4-isopropoxyphenyl)propan-2-one
反応式
Cl.[CH:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[C:13]([N+]([O-])=O)[CH3:14])=[CH:8][CH:7]=1)([CH3:4])[CH3:3].[O:18]1CCCC1>[Fe]>[CH:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][C:13](=[O:18])[CH3:14])=[CH:8][CH:7]=1)([CH3:4])[CH3:3]参加物
5
実験手順
Concentrated hydrochloric acid (90 ml) was added dropwise, over 45 minutes, to a stirred mixture of iron powder (17.5 g) and 1-(4-isopropoxyphenyl)-2-nitroprop1-ene (16.0 g) in tetrahydrofuran (50 ml) at reflux. The mixture was heated under reflux for a further hour, cooled, filtered through diatomaecous earth and the tetrahydrofuran removed under reduced pressure. The residue was diluted with water, extracted with diethyl ether, washed with brine, dried (magnesium sulphate), filtered and evaporated to dryness. Distillation of the residue gave the title compound, bp 120°-6°/1.5 mm.
後処理
- temperatureat reflux
- temperatureThe mixture was heated
- temperatureunder reflux for a further hour
- temperaturecooled
- filtrationfiltered through diatomaecous earth
- customthe tetrahydrofuran removed under reduced pressure
- additionThe residue was diluted with water
- extractionextracted with diethyl ether
- washwashed with brine
- dry with materialdried (magnesium sulphate)
- filtrationfiltered
- customevaporated to dryness
- distillationDistillation of the residue
出典と根拠
- ORDレコード
- ord-c20dbfec2e004b3f8259191b0db34ffc
- 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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