Nitric Acid → N-(5-chloro-4-fluoro-2-nitrophenyl)acetamide
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8].[N+:13]([O-])([OH:15])=[O:14]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:12])[CH3:11])[C:5]([N+:13]([O-:15])=[O:14])=[CH:6][C:7]=1[F:8]参加物
4
実験手順
To a solution of N-(3-chloro-4-fluorophenyl)acetamide (55 g) in concentrated sulfuric acid (165 ml) was added dropwise concentrated nitric acid (d 1.42, 154 ml) at 5°-10° C. during an hour with stirring in an ice-salt bath. After stirring for an hour at the same temperature, the reaction mixture was poured into ice water. The resulting precipitate was collected by filtration, sufficiently washed with water and recrystallized from acetonitrile to give the title compound (48.9 g) as yellow needles, mp 114°-115° C.
後処理
- stirringAfter stirring for an hour at the same temperature
- filtrationThe resulting precipitate was collected by filtration
- washsufficiently washed with water
- customrecrystallized from acetonitrile
出典と根拠
- ORDレコード
- ord-9e29a83732db4959a8020002b024b850
- 出典データセット
- uspto-grants-1989_05
- 特許番号
- US04826982
反応ノート
読み込み中…