Dimethylformamide → 4-Amino-5-ethoxy-2-fluorobenzoic acid
反応式
[CH2:1]([O:3][C:4]1[C:5]([N+:14]([O-])=O)=[CH:6][C:7]([F:13])=[C:8]([CH:12]=1)[C:9]([OH:11])=[O:10])[CH3:2].CN(C=O)C>C(O)C.[Pd]>[NH2:14][C:5]1[C:4]([O:3][CH2:1][CH3:2])=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[C:7]([F:13])[CH:6]=1参加物
5
実験手順
5-ethoxy-2-fluoro-4-nitrobenzoic acid (Intermediate 172; 1.24 g, 5.40 mmol) was stirred and dissolved in ethanol:DMF (50 mL:5 mL) over 5% Pd/C (125 mg) and hydrogenated at ambient temperature for 4 hours. The catalyst was filtered and washed with ethanol and the solvent evaporated. The resultant material was purified on a silica column, eluting with 0-5% MeOH/DCM. Product containing fractions were combined and evaporated to yield the title compound as a pale brown solid (433 mg, 40%)
後処理
- filtrationThe catalyst was filtered
- washwashed with ethanol
- customthe solvent evaporated
- customThe resultant material was purified on a silica column
- washeluting with 0-5% MeOH/DCM
- additionProduct containing fractions
- customevaporated
出典と根拠
- ORDレコード
- ord-43c4891465bf4f35aac60f37de798089
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07709471B2
反応ノート
読み込み中…