3-Nitro-4-phenyl-5-sulfamylbenzoic acid → 3-Amino-4-phenyl-5-sulfamylbenzoic acid
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([S:19](=[O:22])(=[O:21])[NH2:20])[C:12]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]([OH:9])=[O:8])([O-])=O>C(O)(=O)C.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([S:19](=[O:22])(=[O:21])[NH2:20])[C:12]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]([OH:9])=[O:8]参加物
4
実験手順
To a solution of 3-nitro-4-phenyl-5-sulfamylbenzoic acid (8.5 g) in acetic acid (100 ml), palladium (10%) on carbon (1.5 g) is added, and the mixture is hydrogenated. After 2-2.5 hours the theoretical amount of hydrogen has been absorbed, and the hydrogen uptake has subsided. The catalyst is removed by filtration, and the filtrate is evaporated in vacuo. The residue is recrystallized from acetic acid to give 3-amino-4-phenyl-5-sulfamylbenzoic acid with a melting point of 232.5°-237° C.
後処理
- customAfter 2-2.5 hours the theoretical amount of hydrogen has been absorbed
- customThe catalyst is removed by filtration
- customthe filtrate is evaporated in vacuo
- customThe residue is recrystallized from acetic acid
出典と根拠
- ORDレコード
- ord-8cf6a0da7ddb42d4960d7d943f93761f
- 出典データセット
- uspto-grants-1976_04
- 特許番号
- US03950380
反応ノート
読み込み中…