2-(1-Methylethoxy)-5-nitrobenzoic acid → 5-Amino-2-isopropoxybenzoic acid
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-8226a06bf1a54932ac3e629aad9e3ab9
- 출처 데이터셋
- uspto-grants-2013_05
- 특허 번호
- US08450506B2
반응 노트
불러오는 중…