Iodoethane → HCID 20360292、化合物
反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:7]([C:8]([NH2:10])=[O:9])[C:6]([OH:12])=[CH:5][CH:4]=1.I[CH2:14][CH3:15]>[Na].C(O)C>[CH2:14]([O:12][C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:11][C:7]=1[C:8]([NH2:10])=[O:9])[CH3:15]参加物
5
実験手順
5-Methoxysalicylamide (41.8 g., 0.250 mole) was dissolved in a solution of sodium (6.37 g., 0.277 g-atom) in ethanol (250 ml.). To the resulting cooled (ice-water) solution was added iodoethane (38.9 g., 0.250 mole) over a period of 20 minutes. The reaction mixture was allowed to warm to room temperature over 0.75 hour and then was heated under reflux for 19 hours. The mixture was concentrated and the residue triturated with water. The mixture was filtered and the collected solid recrystallized from acetonitrile to give 2-ethoxy-5-methoxybenzamide (34.5 g., 70.7%), m.p. 128°-130°.
後処理
- temperaturewas heated
- temperatureunder reflux for 19 hours
- concentrationThe mixture was concentrated
- customthe residue triturated with water
- filtrationThe mixture was filtered
- customthe collected solid recrystallized from acetonitrile
出典と根拠
- ORDレコード
- ord-ad69d442637b4842a45739cba7f6e3d0
- 出典データセット
- uspto-grants-1978_04
- 特許番号
- US04082751
反応ノート
読み込み中…