3-Chloro-4-(trifluoromethyl)benzyl alcohol → 3-Chloro-4-(trifluoromethyl)benzaldehyde
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])[CH2:5][OH:6]>ClCCCl.O=[Mn]=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[C:10]([F:11])([F:12])[F:13])[CH:5]=[O:6]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Step A A mixture of 3-chloro-4-(trifluoromethyl)benzyl alcohol (Synquest) (4.77 g, 23 mmol) and activated MnO2 (19.5 g, 230 mmol) in 1,2-dichlorethane (80 mL) was heated and stirred at 80° C. for 3 h. The mixture was cooled to room temperature and filtered through a short pad of celite. The celite was washed with dichloromethane, and ethyl acetate. The filtrates were combined, concentrated, dried under reduced pressure to give 3-chloro-4-(trifluoromethyl)benzaldehyde as a light yellow oil (2.8 g, 60%).
後処理
- temperaturewas heated
- temperatureThe mixture was cooled to room temperature
- filtrationfiltered through a short pad of celite
- washThe celite was washed with dichloromethane, and ethyl acetate
- concentrationconcentrated
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-86b6bde40e0747a296759688ef21f51e
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08354444B2
反応ノート
読み込み中…