Ammonium formate → Ethyl 3-amino-2-hydroxybenzoate
反応式
[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-])=O)[C:6]=1[OH:14])[CH3:2].[H][H].C([O-])=O.[NH4+]>CO.[Pd]>[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([NH2:11])[C:6]=1[OH:14])[CH3:2]参加物
6
実験手順
To a solution of 2-hydroxy-3-nitrobenzoic acid ethyl ester 8.4 g (40 mmol) of step 1 in methanol 100 mL was added 5% Pd/C 0.84 g, after which the reactor was filled hydrogen gas, followed by stirring at room temperature for 5 hrs. Ammoniumformate 0.5 g was added to the reaction mixture before re-filling with hydrogen gas and re-stirring at room temperature for 24 hrs. The catalyst was removed by celite filtration, followed by vacuum concentration to afford the title compound 7.2 g (yield 99%).
後処理
- stirringre-stirring at room temperature for 24 hrs
- customThe catalyst was removed by celite filtration
- concentrationfollowed by vacuum concentration
出典と根拠
- ORDレコード
- ord-b8fdd6f131f24842af3a96005482d925
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026235B1
反応ノート
読み込み中…