Hydrochloric Acid → 1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxylic acid
反応式
[CH3:1][N:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH:6]([C:11]([O-:13])=[O:12])[C:5]=2[CH:4]=[N:3]1.[Li+].[OH-].Cl>CO.C1COCC1.O>[CH3:1][N:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH:6]([C:11]([OH:13])=[O:12])[C:5]=2[CH:4]=[N:3]1参加物
7
実験手順
To a solution of 1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxylate (7 g, 36 mmol) in methanol (100 mL), THF (50 mL) and H2O (50 mL) was added LiOH (2.5 g, 108 mmol). The resulting mixture was stirred at room temperature for 2 hours. The reaction mixture was acidified with 1N HCl solution to pH=5-6, and extracted with EA three times. The combined organic layers were washed with brine, dried over Na2SO4. The solvent was concentrated to give 1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxylic acid (6 g, 94%), which was used in the next step directly.
後処理
- extractionextracted with EA three times
- washThe combined organic layers were washed with brine
- dry with materialdried over Na2SO4
- concentrationThe solvent was concentrated
出典と根拠
- ORDレコード
- ord-fd084183767c4a3fbb410b56931aa556
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09446130B2
反応ノート
読み込み中…
