Ammonium Hydroxide → 1H-pyrrolo(2,3-b)pyridin-5-amine
反応式
Br[C:2]1[CH:3]=[C:4]2[CH:10]=[CH:9][NH:8][C:5]2=[N:6][CH:7]=1.[OH-].[NH4+:12]>CCOC(C)=O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2]>[NH:8]1[C:5]2=[N:6][CH:7]=[C:2]([NH2:12])[CH:3]=[C:4]2[CH:10]=[CH:9]1参加物
5
実験手順
5-bromo-1H-pyrrolo[2,3-b]pyridine (6.0 g, 30.45 mmol) in ammonium hydroxide (120 mL) was treated with copper sulphate pentahydrate (1.50 g, 6.09 mmol, 0.2 eq) and heated in a sealed tube overnight. The reaction was diluted with EtOAc and the insoluble black solid was filtered off. The filtrate was extracted (EtOAc/Water) and the organic layer washed with saturated aqueous ammonium chloride, followed by water and brine. The organics were dried over magnesium sulphate, filtered and evaporated to dryness to give the product as a pale brown solid (2.57 g, 63%)
後処理
- temperatureheated in a sealed tube overnight
- filtrationthe insoluble black solid was filtered off
- extractionThe filtrate was extracted (EtOAc/Water)
- washthe organic layer washed with saturated aqueous ammonium chloride
- dry with materialThe organics were dried over magnesium sulphate
- filtrationfiltered
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-3922a1d6c350499993d460cc3cc0efb4
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530489B2
反応ノート
読み込み中…