Methanol → methyl 5-chloro-1H-pyrrolo[3,2-b]pyridine-2-carboxylate
反応式
[Cl:1][C:2]1[N:7]=[C:6]2[CH:8]=[C:9]([C:11]([OH:13])=[O:12])[NH:10][C:5]2=[CH:4][CH:3]=1.S(=O)(=O)(O)O.[CH3:19]O>>[Cl:1][C:2]1[N:7]=[C:6]2[CH:8]=[C:9]([C:11]([O:13][CH3:19])=[O:12])[NH:10][C:5]2=[CH:4][CH:3]=1参加物
4
実験手順
5-chloro-1H-pyrrolo[3,2-b]pyridine-2-carboxylic acid 11-b (25.20 g, 128.18 mmol) was added to a refluxing mixture of sulfuric acid (20 ml) and methanol (400 ml). The mixture was refluxed overnight. The mixture was then evaporated and a cold NaHCO3 solution was added until basic pH. The precipitate was filtered off and dried, yielding 16.15 g of the desired product (59.8%). m/z=211.17 (M+H)+, Cl pattern.
後処理
- temperatureThe mixture was refluxed overnight
- customThe mixture was then evaporated
- additiona cold NaHCO3 solution was added until basic pH
- filtrationThe precipitate was filtered off
- customdried
出典と根拠
- ORDレコード
- ord-2380255430824e29986382e6599250d7
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09339494B2
反応ノート
読み込み中…