Potassium Hydroxide → HCID 22258169、化合物
反応式
[Br:1][C:2]1[N:6]2[C:7](Cl)=[CH:8][CH:9]=[C:10]([C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[O:12])[C:5]2=[N:4][CH:3]=1.[OH-:20].[K+]>C(O)C>[C:11]([C:10]1[CH:9]=[CH:8][C:7](=[O:20])[N:6]2[C:2]([Br:1])=[CH:3][NH:4][C:5]=12)(=[O:12])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1参加物
4
実験手順
40 mg (0.12 mmol) of 3-bromo-5chloroimidazo[1,2-a]pyridin-8-yl)(phenyl)methanone (example L) are dissolved in 5 ml of potassium hydroxide—solution (10% in water) and 5 ml of ethanol. The mixture is stirred for 24 h at rt. The solvent is evaporated under vacuum and water is added to the crude. The solution is extracted for with ethyl acetate. The collected organic phases are reextracted with brine solution and dried over sodium sulfate. The solvent is evaporated under vacuum and the crude is purified over preparative HPLC (RP18-Column, eluent: acetonitrilewater-gradient) to yield 1.6 mg (4.2% of th.) 8-Benzoyl-3-bromoimidazo[1,2-a]pyridin-5(1H)-one.
後処理
- customThe solvent is evaporated under vacuum and water
- additionis added to the crude
- extractionThe solution is extracted for with ethyl acetate
- dry with materialdried over sodium sulfate
- customThe solvent is evaporated under vacuum
- customthe crude is purified over preparative HPLC (RP18-Column, eluent: acetonitrilewater-gradient)
出典と根拠
- ORDレコード
- ord-260ac36685df41e3966a86263b03f220
- 出典データセット
- uspto-grants-2006_01
- 特許番号
- US06984646B2
反応ノート
読み込み中…