Methyl iodide → 3-Bromo-5-chloro-1-methylpyridin-2(1H)-one
반응식
[Br:1][C:2]1[C:3](=[O:9])[NH:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.[C:10](=O)([O-])[O-].[K+].[K+].IC>COCCOC>[Br:1][C:2]1[C:3](=[O:9])[N:4]([CH3:10])[CH:5]=[C:6]([Cl:8])[CH:7]=1참가 물질
5
실험 절차
A mixture of 3-bromo-5-chloro-1H-2-pyridone (930 mg, 4.46 mmol), potassium carbonate (1.25 g, 9.1 mmol) and iodomethane (2.8 mL, 45 mmol) in 10 mL of DME was heated to reflux for 18 hr. The mixture was filtered hot and concentrated. The residue was recrystallized from ethyl acetate to give 3-bromo-5-chloro-1-methyl-2-pyridone (740 mg, 74%), mp 162-163° C. HRMS (C6H5BrClNO): Obs. Mass 220.9249. Calcd. Mass 220.9243 (M+H).
후처리
- temperaturewas heated
- temperatureto reflux for 18 hr
- filtrationThe mixture was filtered hot
- concentrationconcentrated
- customThe residue was recrystallized from ethyl acetate
출처 및 근거
- ORD 기록
- ord-9da37b386b744036a22fd1306271d042
- 출처 데이터셋
- uspto-grants-2005_07
- 특허 번호
- US06916933B2
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