反応式
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([NH2:11])[CH:3]=1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>O>[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([NH:11][C:12](=[O:14])[CH3:13])[CH:3]=1参加物
4
反応条件
- 温度
- 130 °C
実験手順
4-Methyl-5-nitro-2-pyridinamine (3.69 g, 2.41 mmol) was added with acetic anhydride (10 ml) and stirred at 130° C. for 1.5 hours. The reaction mixture was left stand for cooling, and then added with distilled water (5.4 ml) at 0° C., heated to 130° C., and stirred for 45 minutes. The reaction mixture was left stand for cooling and concentrated, and the deposited crystals were collected by filtration and washed with distilled water to obtain the title compound (4.71 g, quantitative).
後処理
- waitThe reaction mixture was left stand
- temperaturefor cooling
- temperatureheated to 130° C.
- stirringstirred for 45 minutes
- waitThe reaction mixture was left stand
- temperaturefor cooling
- concentrationconcentrated
- filtrationthe deposited crystals were collected by filtration
- washwashed with distilled water
出典と根拠
- ORDレコード
- ord-ae1dc800dc2640f1a468cc2b45daad5f
- 出典データセット
- uspto-grants-2006_06
- 特許番号
- US07056917B2
関連ノート
読み込み中…