反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH:12](O)[CH2:13][N+:14]([O-:16])=[O:15])[CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.C(N(CC)CC)C>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2(/[CH:12]=[CH:13]/[N+:14]([O-:16])=[O:15])[CH2:9][CH2:10][CH2:11]2)=[CH:6][CH:7]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
1-(1-(4-Chlorophenyl)cyclobutyl)-2-nitroethanol (5.2 g, 20.34 mmol) was dissolved in dichloromethane (41 ml) and trifluoroacetic acid anhydride (2.87 ml, 20.34 mmol) was added. The reaction mixture was cooled to 0° C. and triethylamine (5.67 ml, 40.7 mmol) was added dropwise. The reaction was slowly warmed to room temperature and stirring Was continued for 2 h. The reaction mixture was diluted with dichloromethane and washed with aqueous hydrochloric acid (1 N). The organic layer was dried (magnesium sulfate) and concentrated in vacuo. The crude product was purified by flash chromatography (silica, dichloromethane, methanol). Yield: 3.99 g (16.79 mmol, 83%)
後処理
- temperatureThe reaction was slowly warmed to room temperature
- washwashed with aqueous hydrochloric acid (1 N)
- dry with materialThe organic layer was dried (magnesium sulfate)
- concentrationconcentrated in vacuo
- customThe crude product was purified by flash chromatography (silica, dichloromethane, methanol)
出典と根拠
- ORDレコード
- ord-0d12ee125a564d98892a285f8e239deb
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877794B2
関連ノート
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