反応式
C([O:8][C:9]1[C:14]([Cl:15])=[CH:13][C:12]([NH:16][C:17]2[CH:26]=[CH:25][CH:24]=[CH:23][C:18]=2[C:19]([O:21][CH3:22])=[O:20])=[CH:11][C:10]=1[Cl:27])C1C=CC=CC=1>[Pd].C1COCC1>[Cl:15][C:14]1[CH:13]=[C:12]([NH:16][C:17]2[CH:26]=[CH:25][CH:24]=[CH:23][C:18]=2[C:19]([O:21][CH3:22])=[O:20])[CH:11]=[C:10]([Cl:27])[C:9]=1[OH:8]参加物
4
実験手順
Palladium on carbon (10% by mass of 10% by wt Pd, 50 mg) was cautiously added to a deoxygenated stirring solution of methyl 2-(4-(benzyloxy)-3,5-dichlorophenylamino)benzoate (0.520 g, 1.3 mmol) in THF (15 mL). The mixture was subjected to three cycles of evacuation and purging with hydrogen gas, before being stirred under an atmosphere of hydrogen gas. After 3 h, the reaction was purged with nitrogen, filtered through Celite™ (eluent: THF) and concentrated in vacuo to afford methyl 2-(3,5-dichloro-4-hydroxyphenylamino)benzoate as a white solid that was used without further purification.
後処理
- custompurging with hydrogen gas
- customthe reaction was purged with nitrogen
- filtrationfiltered through Celite™ (eluent: THF)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-7bde8d590a624b9e8e29c4ca16a04b98
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08236984B2
関連ノート
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