Bromine → HCID 19079294、化合物
反応式
[Br:1]Br.[CH3:3][N:4]1[C:8]2=[N:9][CH:10]=[C:11]([C:13](=[O:15])[CH3:14])[CH:12]=[C:7]2[CH2:6][C:5]1=[O:16]>C(O)(=O)C>[Br:1][CH2:14][C:13]([C:11]1[CH:12]=[C:7]2[CH2:6][C:5](=[O:16])[N:4]([CH3:3])[C:8]2=[N:9][CH:10]=1)=[O:15]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Add 170 mg (1.05 mmol) of bromine dissolved in 1 ml of acetic acid dropwise to a solution of 200 mg (1.05 mmol) of 1,3-dihydro-1-methyl-5-acetyl-2H-pyrrolo[2,3-b]pyridin-2-one (obtained as described in Example 13 hereinafter) in 4 ml of acetic acid. After 6 hours' heating at 80° C., the acetic acid is removed under reduced pressure and the residue is taken up in water and then extracted with dichloromethane. The crude product obtained is purified by chromatography on silica gel (eluant ethyl acetate/petroleum ether/dichloromethane, 1/1/1).
後処理
- customthe acetic acid is removed under reduced pressure
- extractionextracted with dichloromethane
出典と根拠
- ORDレコード
- ord-b1e0dfa340284d7c9c321e2e787a0f02
- 出典データセット
- uspto-grants-1998_06
- 特許番号
- US05767128
反応ノート
読み込み中…