Phosphorus oxychloride → 2-Chloroisonicotinic acid
反応式
P(Cl)(Cl)([Cl:3])=O.[C:6]([OH:15])(=[O:14])[C:7]1[CH:12]=[CH:11][N+:10]([O-])=[CH:9][CH:8]=1>>[Cl:3][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][N:10]=1)[C:6]([OH:15])=[O:14]参加物
3
反応条件
- 温度
- 120 °C
実験手順
Phosphorus oxychloride (220.7 g) was added to isonicotinic acid N-oxide (50.064 g), and the mixture was stirred on an oil bath at 120° C. for 7 hours. The reaction mixture was slowly poured into ice water with vigorously stirring to precipitate light yellow crystals. The mixture was adjusted to approximately pH 4 with 4N NaOH aqueous solution. The resulting crystals were filtered out, washed with water, and dried by vacuum heating (60° C.) to obtain the above-captioned compound ([9]-(92)-467) (37.845 g).
後処理
- stirringwith vigorously stirring
- customto precipitate light yellow crystals
- filtrationThe resulting crystals were filtered out
- washwashed with water
- customdried by vacuum
- temperatureheating (60° C.)
- customto obtain the above-captioned compound ([9]-(92)-467) (37.845 g)
出典と根拠
- ORDレコード
- ord-8debf37587f1426b9a2fd8782e5c9316
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05731310
反応ノート
読み込み中…