Hydrochloric Acid → 1-(1-Methyl-1H-pyrazol-4-yl)-2-piperazinone
反応式
[CH3:1][N:2]1[CH:6]=[C:5]([N:7]2[CH2:12][CH2:11][N:10](C(OC(C)(C)C)=O)[CH2:9][C:8]2=[O:20])[CH:4]=[N:3]1.Cl>C(OCC)(=O)C>[CH3:1][N:2]1[CH:6]=[C:5]([N:7]2[CH2:12][CH2:11][NH:10][CH2:9][C:8]2=[O:20])[CH:4]=[N:3]1参加物
4
反応条件
- 温度
- 0 °C
実験手順
tert-Butyl 4-(1-methyl-1H-pyrazol-4-yl)-3-oxopiperazine-1-carboxylate (0.058 g, 0.21 mmol) was suspended in ethyl acetate (2 mL), cooled to 0° C., and saturated with gaseous hydrogen chloride. The mixture was warmed to ambient temperature and after 18 hours, concentrated in vacuo. The mixture was treated with sodium bicarbonate (aqueous saturated), washed with a 10% solution of methanol in dichloromethane (3×), filtered, and concentrated in vacuo, providing the titled.
後処理
- temperatureThe mixture was warmed to ambient temperature and after 18 hours
- concentrationconcentrated in vacuo
- additionThe mixture was treated with sodium bicarbonate (aqueous saturated)
- washwashed with a 10% solution of methanol in dichloromethane (3×)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customproviding the
出典と根拠
- ORDレコード
- ord-03a10d14147d480282fb635f1ec82d8f
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08507494B2
反応ノート
読み込み中…