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[CH3:1][O:2][C:3]1[CH:7]=[C:6]([C:8]([O:10]C)=[O:9])[N:5]([CH3:12])[N:4]=1.[OH-].[Na+].Cl>CO>[CH3:1][O:2][C:3]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[N:5]([CH3:12])[N:4]=1참가 물질
실험 절차
To a solution of methyl 3-methoxy-1-methyl-1H-pyrazole-5-carboxylate (2.01 g, 11.8 mmol) in methanol (15 mL) was added 8N aqueous sodium hydroxide solution (3.00 mL), and the mixture was stirred at room temperature for 18 hr. 6N Hydrochloric acid (4.00 mL) was added to the mixture, and the mixture was concentrated under reduced pressure. Water was added to the residue, and the precipitate was collected by filtration, washed with water and air-dried. The precipitate was suspended in diisopropyl ether, and the mixture was stirred at 80° C. for 15 min. After allowing to cool to room temperature, the precipitate was collected by filtration, washed with diisopropyl ether, and dried under reduced pressure to give the title compound (746 mg, yield 40%) as a white solid.
후처리
- concentrationthe mixture was concentrated under reduced pressure
- additionWater was added to the residue
- filtrationthe precipitate was collected by filtration
- washwashed with water
- customair-dried
- stirringthe mixture was stirred at 80° C. for 15 min
- temperatureto cool to room temperature
- filtrationthe precipitate was collected by filtration
- washwashed with diisopropyl ether
- customdried under reduced pressure
출처 및 근거
- ORD 기록
- ord-3b0193f58f91438798db370e0b6db7f9
- 출처 데이터셋
- uspto-grants-2011_10
- 특허 번호
- US08034812B2
연결된 노트
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