Pyridinium hydrobromide → 4-bromo-5-methoxypyridin-2(1H)-one
反応式
Br.[NH+]1C=CC=CC=1.[Br:8][C:9]1[C:14]([O:15][CH3:16])=[CH:13][N:12]=[C:11]([O:17]C)[CH:10]=1>CN(C)C=O>[Br:8][C:9]1[C:14]([O:15][CH3:16])=[CH:13][NH:12][C:11](=[O:17])[CH:10]=1参加物
4
反応条件
- 温度
- 100 °C
実験手順
2.82 g (176 mmol, 20 eq.) of pyridinium hydrobromide were added to a solution of 1.94 g (8.81 mmol) of 4-bromo-2,5-dimethoxypyridine in 80 ml of dimethylformamide, the mixture was stirred at 100° C. for 3 h and concentrated under reduced pressure. The residue was triturated with 50 ml of water, filtered off, washed with water and dried under reduced pressure. The filtrate was extracted twice with dichloromethane/methanol (10:1). The combined organic phases were dried (sodium sulphate), filtered, concentrated under reduced pressure and dried. Yield: 771 mg (43% of theory) and 465 mg (purity 88%, 23% of theory)
後処理
- concentrationconcentrated under reduced pressure
- customThe residue was triturated with 50 ml of water
- filtrationfiltered off
- washwashed with water
- customdried under reduced pressure
- extractionThe filtrate was extracted twice with dichloromethane/methanol (10:1)
- dry with materialThe combined organic phases were dried (sodium sulphate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customdried
出典と根拠
- ORDレコード
- ord-30975c292b814143a149ac6091aa4b33
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434690B2
反応ノート
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