Phosphorus oxychloride → 7-Chloro-3,5-dimethylisoxazolo[4,5-b]pyridine
反応式
[CH3:1][C:2]1[C:6]2=[N+:7]([O-])[C:8]([CH3:11])=[CH:9][CH:10]=[C:5]2[O:4][N:3]=1.O=P(Cl)(Cl)[Cl:15].C([O-])(O)=O.[Na+]>C(Cl)(Cl)Cl>[Cl:15][C:10]1[CH:9]=[C:8]([CH3:11])[N:7]=[C:6]2[C:2]([CH3:1])=[N:3][O:4][C:5]=12参加物
5
反応条件
- 温度
- 80 °C
実験手順
3,5-dimethylisoxazolo[4,5-b]pyridine 4-oxide (0.650 g, 3.96 mmol) in chloroform (5 mL), was added POCl3 (1.45 mL, 15.8 mmol) and the mixture was heated at 80° C. for 2 hours. The solution was cooled and poured onto ice water. The solution was neutralized with saturated NaHCO3 and the solution was then extracted with EtOAc, dried, and concentrated. The solid was triturated with ether and filtered twice to obtain two crops of the title compound (0.417 g, 57.7% yield).
後処理
- temperatureThe solution was cooled
- additionpoured onto ice water
- extractionthe solution was then extracted with EtOAc
- customdried
- concentrationconcentrated
- customThe solid was triturated with ether
- filtrationfiltered twice
出典と根拠
- ORDレコード
- ord-ff9ef4ad650b41b7bee7f5e52f90b563
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08354540B2
反応ノート
読み込み中…