Nitroethane → 2,4-Dichloro-1-(2-nitro-1-propen-1-yl)benzene
反応式
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.C([O-])(=O)C.[NH4+].[N+:16]([CH2:19][CH3:20])([O-:18])=[O:17]>C(OCC)(=O)C>[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=[C:19]([N+:16]([O-:18])=[O:17])[CH3:20]参加物
5
実験手順
A mixture of 2,4-dichlorobenzaldehyde (1.45 g, 8.3 mmol), ammonium acetate (0.64 g, 8.3 mmol) and nitroethane (6 g, 80 mmol) was heated under reflux for 6 hr. The mixture was allowed to cool to room temperature and ethyl acetate was added. The mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated. Recrystallization from ethanol gave 2,4-dichloro-1-(2-nitro-1-propenyl)benzene (yellow needle crystals, yield; 1.0 g, 52%).
後処理
- temperaturewas heated
- temperatureunder reflux for 6 hr
- washThe mixture was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customRecrystallization from ethanol
出典と根拠
- ORDレコード
- ord-1399554a04494fd9a666bf997f38615d
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08378114B2
反応ノート
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