Acetic Anhydride → (3-Methylpyridin-4-yl)methyl acetate
反応式
[N+:1]1([O-])[CH:6]=[CH:5][C:4]([CH3:7])=[C:3]([CH3:8])[CH:2]=1.[C:10]([O:13]C(=O)C)(=[O:12])[CH3:11]>O>[C:10]([O:13][CH2:7][C:4]1[CH:5]=[CH:6][N:1]=[CH:2][C:3]=1[CH3:8])(=[O:12])[CH3:11]参加物
4
実験手順
The N-oxide was added portionwise to 60 mL of acetic anhydride and the resulting dark orange solution was heated (water-bath) at about 90° C. for 1 h. The excess acetic anhydride was then distilled off under reduced pressure and the material boiling at 90°-120° C./0.1 torr (39.0 g) was collected. Chromatography of this oil (silica gel/ethyl acetate-pet.ether=2:3) afforded pure 4-acetoxymethyl-3-methylpyridine (19.0 g, 30%) as an oil: ir (neat) 1745 cm-1.
後処理
- distillationThe excess acetic anhydride was then distilled off under reduced pressure
- customthe material boiling at 90°-120° C./0.1 torr (39.0 g) was collected
出典と根拠
- ORDレコード
- ord-4733ba85c7be43ba8ce4561e8017e9af
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04644061
反応ノート
読み込み中…