Methyl iodide → 3-Methoxy-1-methylpyridin-2-one
反応式
[CH3:1][O:2][C:3]1[C:4](=[O:9])[NH:5][CH:6]=[CH:7][CH:8]=1.[OH-].[K+].[CH3:12]I>CO>[CH3:12][N:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]1=[O:9]参加物
5
実験手順
A mixture of 3-methoxy-2(1H)-pyridone (25 g., 0.2 moles), potassium hydroxide (16 g., 0.24 moles) and methyl iodide (45.4 g., 0.32 moles) in 400 ml. methanol is heated at reflux for 5 hours. The methanol is removed under reduced pressure leaving a solid redidue which is extracted with methylene chloride. The methylene chloride extracts are washed with water, a saturated salt solution, and dried over sodium sulfate. Evaporation of the dried extracts, under reduced pressure, affords 1-methyl-3-methoxy-2(1H)-pyridone as a colorless oil which solidifies on standing (26.2 g., 94%). The pyridone is very hygroscopic and rapidly liquifies on exposure to air.
後処理
- temperatureat reflux for 5 hours
- customThe methanol is removed under reduced pressure
- customleaving a solid redidue which
- extractionis extracted with methylene chloride
- washThe methylene chloride extracts are washed with water
- dry with materiala saturated salt solution, and dried over sodium sulfate
- customEvaporation of the dried extracts
出典と根拠
- ORDレコード
- ord-14fbee2fa7ed4ca0bea4dcb2924b3026
- 出典データセット
- uspto-grants-1976_05
- 特許番号
- US03957997
反応ノート
読み込み中…