反応 #736391

反応方程式

3-Methoxy-2-methyl-4(1H)-pyridone

phosphorus oxychloride

→

4-chloro-3-methoxy-2-methylpyridine

反応条件

後処理

1. 1
   温度refluxed for 10 hours
2. 2
   濃縮concentrated
3. 3
   workup.ADDITIONTo the resultant residue was added toluene
4. 4
   その他the residual phosphorus oxychloride was evaporated under reduced pressure
5. 5
   workup.ADDITIONTo the resultant oily substance were added chloroform and water
6. 6
   その他the chloroform layer was separated
7. 7
   抽出extracted with chloroform
8. 8
   その他The chloroform solutions thus obtained
9. 9
   洗浄washed with water
10. 10
    その他dried
11. 11
    その他evaporated
12. 12
    その他The residue was purified by column chromatography on silica gel

実験手順

3-Methoxy-2-methyl-4(1H)-pyridone (5.6 g) was suspended in phosphorus oxychloride (50 ml), refluxed for 10 hours, and concentrated. To the resultant residue was added toluene and the residual phosphorus oxychloride was evaporated under reduced pressure. To the resultant oily substance were added chloroform and water and the chloroform layer was separated. The aqueous layer was made alkaline with potassium carbonate and extracted with chloroform. The chloroform solutions thus obtained were combined, washed with water, dried, and evaporated. The residue was purified by column chromatography on silica gel, to give 4-chloro-3-methoxy-2-methylpyridine (4.8 g) as a light brown oil.

出典