Pyridinium hydrobromide → 4-bromo-5-methoxypyridin-2(1H)-one
반응식
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]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
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)
후처리
- 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
출처 및 근거
- ORD 기록
- ord-30975c292b814143a149ac6091aa4b33
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434690B2
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