Ethanol → 2,6-Dichloro-3,5-dimethoxyaniline
反応式
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([Cl:12])[C:3]=1[NH:13]C(=O)C.CCO.[OH-].[K+]>O>[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([Cl:12])[C:3]=1[NH2:13]参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a suspension of N-(2,6-Dichloro-3,5-dimethoxy-phenyl)-acetamide 15 (6.50 g, 24.61 mmol) in mixture of EtOH (80 mL) and water (30 mL), is added KOH (20 g) and stirred 2 days at 80° C. After the solvent (EtOH) is removed on vacuum, water (˜15 mL) is added, a white solid is collected by filtration and washed with water, dried to give final product 16: 1H NMR 600 MHz (CDCl3) δ 6.03 (s, 1H), 4.55 (s, 2H), 3.88 (s, 6H); MS m/z 222.00 (M+1).
後処理
- customAfter the solvent (EtOH) is removed on vacuum, water (˜15 mL)
- additionis added
- filtrationa white solid is collected by filtration
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-6d06e9a29f3743f6bd7dc7dc17c6ee2a
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026243B2
反応ノート
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