Methyl iodide → 3-Bromo-5-chloro-1-methylpyridin-2(1H)-one
反応式
[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]=1参加物
5
実験手順
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).
後処理
- temperaturewas heated
- temperatureto reflux for 18 hr
- filtrationThe mixture was filtered hot
- concentrationconcentrated
- customThe residue was recrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-9da37b386b744036a22fd1306271d042
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06916933B2
反応ノート
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