Hydrochloric Acid → Pyrazole-5-carboxylic acid, 3-phenyl-
反応式
[C:1]1([C:7]2[CH:11]=[C:10]([C:12]([O:14]C)=[O:13])[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li+].[OH-].Cl>C1COCC1.O>[C:1]1([C:7]2[CH:11]=[C:10]([C:12]([OH:14])=[O:13])[NH:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1参加物
6
実験手順
To a solution of methyl 3-phenyl-1H-pyrazole-5-carboxylate (6.02 g, 29.8 mmol) in THF and H2O (3:1, 140 mL) was added LiOH (3.42 g, 142.8 mmol) and the mixture was stirred overnight at room temperature. It was poured into 2N HCl solution (150 mL) and extracted with ethyl acetate. After extration, the organic layer was dried over anhydrous sodium sulfate, filtered and concentrated at reduced pressure to afford product (3.2 g, 57.1%): MS (EI) for C10H8N2O2: 189.26 (MH+).
後処理
- extractionextracted with ethyl acetate
- dry with materialAfter extration, the organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated at reduced pressure
出典と根拠
- ORDレコード
- ord-833b35e2f6e74ff492cf0e0deb503280
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08710038B2
反応ノート
読み込み中…