Hydrochloric Acid → 3-(5-Amino-1-methylpyrazol-4-yl)propylamine dihydrochloride
反応式
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[CH:4][C:3]=1[CH2:8][CH2:9][CH2:10][N:11]1C(=O)C2=CC=CC=C2C1=O.[ClH:22]>O>[ClH:22].[ClH:22].[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[CH:4][C:3]=1[CH2:8][CH2:9][CH2:10][NH2:11]参加物
4
実験手順
5-Amino-1-methyl-4-(3-phthalimidopropyl)pyrazole (1.42 g, 5 mmol) was added to concentrated hydrochloric acid (10 ml) at room temperature, and the mixture was stirred under reflux for 23 hours. To the reaction mixture was added water (50 ml), and most of insoluble materials were removed by filtration. The filtrate was washed with ethyl acetate, and the aqueous layer was concentrated in vacuo. The residue was triturated with 2-propanol and dried in vacuo to give 3-(5-amino-1-methylpyrazol-4-yl)propylamine dihydrochloride (700 mg) as a solid.
後処理
- temperatureunder reflux for 23 hours
- custommost of insoluble materials were removed by filtration
- washThe filtrate was washed with ethyl acetate
- concentrationthe aqueous layer was concentrated in vacuo
- customThe residue was triturated with 2-propanol
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-106e3c25fe28488ab8f6102497abc411
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07179801B2
反応ノート
読み込み中…