Hydrochloric Acid → 2-Amino-5-(propan-2-yl)benzoic acid
반응식
C([NH:4][C:5]1[CH:13]=[CH:12][C:11]([CH:14]([CH3:16])[CH3:15])=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])(=O)C.O.[OH-].[Li+].Cl>C1COCC1.O>[NH2:4][C:5]1[CH:13]=[CH:12][C:11]([CH:14]([CH3:16])[CH3:15])=[CH:10][C:6]=1[C:7]([OH:9])=[O:8]참가 물질
6
실험 절차
A mixture of Example 2B (0.621 g, 2.81 mmol) and lithium hydroxide monohydrate (0.38 g, 9.0 mmol) in THF (6 mL) and water (6 mL) was stirred at 60° C. for 72 hours, acidified to pH 3.5 with 1M HCl, and extracted twice with ethyl acetate. The combined extracts were dried (MgSO4), filtered, and concentrated. The concentrate was purified by C18 reverse-phase HPLC with acetonitrile/water/0.1% TFA to provide the desired product. MS (ESI(+)) m/e 180 (M+H)+; (ESI(−)) m/e 178 (M−H)−.
후처리
- extractionextracted twice with ethyl acetate
- dry with materialThe combined extracts were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe concentrate was purified by C18 reverse-phase HPLC with acetonitrile/water/0.1% TFA
출처 및 근거
- ORD 기록
- ord-c4628c146d214e22821e3d0a42ed2569
- 출처 데이터셋
- uspto-grants-2009_02
- 특허 번호
- US07491718B2
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