Hydrochloric Acid → 2-Amino-1-(3-methoxyphenyl)ethanone
反応式
[N:1]([CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[CH:8]=1)=[O:6])=[N+]=[N-].[ClH:15]>[Pd].CO>[ClH:15].[NH2:1][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[CH:8]=1)=[O:6]参加物
6
反応条件
- 温度
- 25 °C
実験手順
Palladium on carbon (10 wt %, 10.41 g, 9.78 mmol) was added to a solution of 2-azido-1-[3-(methyloxy)phenyl]ethanone (1.87 g, 9.78 mmol) and hydrochloric acid (8.14 mL, 98 mmol) in CH3OH (50 mL) under nitrogen, and the reaction mixture was stirred under hydrogen overnight at 25° C. The mixture was filtered, washing with CH2Cl2 (50 mL) and CH3OH (100 mL), and then concentrated. Water (150 mL) was added, and the mixture was lyophilized to afford an HCl salt of the title compound (2.0 g) as a brown solid. LC-MS (ES) m/z=166 [M+H]+.
後処理
- filtrationThe mixture was filtered
- washwashing with CH2Cl2 (50 mL) and CH3OH (100 mL)
- concentrationconcentrated
- additionWater (150 mL) was added
出典と根拠
- ORDレコード
- ord-ab9fdc775cf34e7b93852829c5416a1a
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08697685B2
反応ノート
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