Hydrazine hydrate (1:1) → Ammonia
반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][CH2:8][C:9]([O:11]CC)=O.O.[NH2:15][NH2:16]>C(O)(C)C>[NH3:1].[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][CH2:8][C:9]([NH:15][NH2:16])=[O:11]참가 물질
5
실험 절차
A mixture of ethyl 2-pyrimidinyloxyacetate (GB2373186, step i ex 368) (4.4 g, 24.15 mmol) and hydrazine hydrate (5 mL, 160 mmol) in isopropanol (30 mL) was heated under reflux for 1 hour. The mixture was then cooled and concentrated under reduced pressure and the residue was purified by column chromatography on silica gel using dichloromethane:methanol:0.88 ammonia (100:0:0 to 100:10:1) to provide the title compound, 600 mg.
후처리
- temperaturewas heated
- temperatureunder reflux for 1 hour
- temperatureThe mixture was then cooled
- concentrationconcentrated under reduced pressure
- customthe residue was purified by column chromatography on silica gel
출처 및 근거
- ORD 기록
- ord-18a1d1b403a64c7798710f754feaa548
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08093400B2
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