2-(1-Methylethoxy)-5-nitrobenzoic acid → 5-Amino-2-isopropoxybenzoic acid
反応式
[CH:1]([O:4][C:5]1[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])([CH3:3])[CH3:2]>CCO.[Pd]>[NH2:14][C:11]1[CH:12]=[CH:13][C:5]([O:4][CH:1]([CH3:3])[CH3:2])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8]参加物
4
実験手順
2-Isopropoxy-5-nitrobenzoic acid (6.02 g, 26.75 mmol) was suspended in EtOH (100 ml) and 10% Pd on C (wet basis) (600 mg) was added. The mixture was hydrogenated at 50 psi for 2 hrs. The mixture was filtered through celite and the volatiles were removed in vacuo. The residue was triturated with IPA, and the resulting solid filtered off, washed with MTBE and dried in vacuo to give 4.15 g of 5-amino-2-isopropoxybenzoic acid (79.5%) as a pale yellow solid.
後処理
- filtrationThe mixture was filtered through celite
- customthe volatiles were removed in vacuo
- customThe residue was triturated with IPA
- filtrationthe resulting solid filtered off
- washwashed with MTBE
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-8226a06bf1a54932ac3e629aad9e3ab9
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08450506B2
反応ノート
読み込み中…