Hydrochloric Acid → 2-Amino-5-(propan-2-yl)benzoic acid
反応式
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]参加物
6
実験手順
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)−.
後処理
- 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
出典と根拠
- ORDレコード
- ord-c4628c146d214e22821e3d0a42ed2569
- 出典データセット
- uspto-grants-2009_02
- 特許番号
- US07491718B2
反応ノート
読み込み中…