Hydrazine → HCID 178487565, 화합물
반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:5]=1F)=O.[NH2:13][NH2:14]>O>[CH3:11][O:10][C:7]1[CH:6]=[C:5]2[C:4]([C:2]([CH3:1])=[N:13][NH:14]2)=[CH:9][CH:8]=1참가 물질
4
실험 절차
2-fluoro-4-methoxyacetophenone (5.0 g) was treated with hydrazine (75 ml) under argon and the mixture was heated to reflux for 12 hours. After cooling to room temperature, the reaction mixture was poured into water (200 ml) then extracted three times with ethyl acetate (50 ml). The combined extracts were dried over sodium sulphate then evaporated. The residue was subjected to flash chromatography on silica eluting with a mixture of ethyl acetate and hexane (1:3, v/v) to yield the title compound (4.05 g).
후처리
- temperaturethe mixture was heated
- temperatureto reflux for 12 hours
- extractionthen extracted three times with ethyl acetate (50 ml)
- dry with materialThe combined extracts were dried over sodium sulphate
- customthen evaporated
- additionThe residue was subjected to flash chromatography on silica eluting with a mixture of ethyl acetate and hexane (1:3
출처 및 근거
- ORD 기록
- ord-7e55a2d6763e428eb20b6a22c94fa28e
- 출처 데이터셋
- uspto-grants-2001_10
- 특허 번호
- US06303600B1
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