Phosphorus oxychloride → HCID 178478308、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[NH:10][C:9](=O)[NH:8][C:5]2=[N:6][CH:7]=1.O=P(Cl)(Cl)[Cl:14]>>[Br:1][C:2]1[CH:3]=[C:4]2[N:10]=[C:9]([Cl:14])[NH:8][C:5]2=[N:6][CH:7]=1参加物
3
実験手順
Reflux 6-bromo-1,3-dihydro-imidazo[4,5-b]pyridin-2-one (5 g) for 14 h in POCl3 (50 mL). Evaporate the solvent in vacuo, then carefully neutralize with saturated NaHCO3, and extract with EtOAc. Dry over Na2SO4, concentrate under vacuum, and purify by flash chromatography (1 :1 hexanes/EtOAc) to obtain 6-bromo-2-chloro-3H-imidazo[4,5-b]pyridine.
後処理
- customEvaporate the solvent in vacuo
- extractionextract with EtOAc
- dry with materialDry over Na2SO4
- concentrationconcentrate under vacuum
- custompurify by flash chromatography (1 :1 hexanes/EtOAc)
出典と根拠
- ORDレコード
- ord-1ab2c821fe32404d9a508e7120e4011c
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06566367B2
反応ノート
読み込み中…