3-Chloropropionyl chloride → 3-chloro-N-(2-fluoro-4-hydroxyphenyl)propanamide
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[F:9].[Cl:10][CH2:11][CH2:12][C:13](Cl)=[O:14]>CC(C)=O>[Cl:10][CH2:11][CH2:12][C:13]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[F:9])=[O:14]参加物
4
実験手順
4-Amino-3-fluorophenol (3.4 g) was mixed with 3-chloropropanoyl chloride (3.56 g) in acetone (60 mL) and heated at reflux over 3 hours. After aqueous work-up with EtOAc/water, the isolated organic layers were dried over Na2SO4 and concentrated in vacuo. The crude product was purified with silica gel chromatography to give the product (2.95 g) as a light brown solid.
後処理
- temperatureheated
- temperatureat reflux over 3 hours
- dry with materialAfter aqueous work-up with EtOAc/water, the isolated organic layers were dried over Na2SO4
- concentrationconcentrated in vacuo
- customThe crude product was purified with silica gel chromatography
出典と根拠
- ORDレコード
- ord-2e11691e25a74dbe9424770cd4a8d518
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09433618B2
反応ノート
読み込み中…