反応式
Cl.[NH2:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].[CH3:14]O>>[NH2:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:4]=1[C:5]([O:7][CH3:14])=[O:6]参加物
4
反応条件
- 温度
- 60 °C
実験手順
Hydrogen chloride gas was bubbled through a solution of 2-amino-5-methoxybenzoic acid (5.0 g, 30 mmol) in MeOH (200 mL) for 30 minutes. The solution was heated at 60° C. overnight. The reaction was cooled and the solvent removed in vacuo. The residue was dissolved in water, basified with 5M NaOH and extracted twice with ether. The ether extracts were washed with 5M NaOH and water, dried (MgSO4), filtered and concentrated in vacuo to give i-e (4.25 g, 78%): MS m/z=182 (M+H).
後処理
- temperatureThe reaction was cooled
- customthe solvent removed in vacuo
- dissolutionThe residue was dissolved in water
- extractionextracted twice with ether
- washThe ether extracts were washed with 5M NaOH and water
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give i-e (4.25 g, 78%)
出典と根拠
- ORDレコード
- ord-7fc8fb3b35f1478b8069aee2cc738136
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07935694B2
関連ノート
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