Hydrochloric Acid → 1-(1-Methyl-1H-pyrazol-4-yl)-2-piperazinone
반응식
[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]1참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-03a10d14147d480282fb635f1ec82d8f
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08507494B2
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