Methyl iodide → 6-Bromo-3-methoxy-2,4-dimethylpyridine
反応式
[Br:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([OH:9])=[C:4]([CH3:10])[CH:3]=1.IC.[C:13](=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Br:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([O:9][CH3:13])=[C:4]([CH3:10])[CH:3]=1参加物
5
実験手順
A mixture of 6-bromo-2,4-dimethyl-3-hydroxypyridine (8.7 g, 43.1 mmol), iodomethane (4.0 mL, 64.6 mmol) and potassium carbonate (11.9 g, 86.1 mmol) in acetone (250 mL) was heated at reflux temperature for 3 hours. The reaction mixture was then cooled to room temperature and filtered through a pad of Celite®. The filtrate was concentrated under reduced pressure and the residue was purified by flash column chromatography using 20% ethyl acetate in hexane to afford 7.9 g (85%) of the title compound.
後処理
- temperaturewas heated
- temperatureat reflux temperature for 3 hours
- filtrationfiltered through a pad of Celite®
- concentrationThe filtrate was concentrated under reduced pressure
- customthe residue was purified by flash column chromatography
出典と根拠
- ORDレコード
- ord-76de05dbfe964f4290e4bd267e8486fe
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08030500B2
反応ノート
読み込み中…