Hydrazine hydrate (1:1) → HCID 178526599、化合物
反応式
C[N:2](C)/[CH:3]=[CH:4]/[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-:15])=[O:14])[CH:8]=1)=O.O.[NH2:18]N>C(O)C>[N+:13]([C:9]1[CH:8]=[C:7]([C:5]2[CH:4]=[CH:3][NH:2][N:18]=2)[CH:12]=[CH:11][CH:10]=1)([O-:15])=[O:14]参加物
4
実験手順
2.5 g (11 mmol) of (2E)-3-(dimethylamino)-1-(3-nitrophenyl)prop-2-en-1-one were dissolved in 25 ml of ethanol and 2.3 ml of hydrazine hydrate 98% (46 mmol) were added. The resulting solution was refluxed under stirring for 5 hours. The solvent was then evaporated and the crude was dissolved with dichloromethane and washed with water. The organic layer was dried over sodium sulphate and the solvent removed in vacuo. The residue was then triturated with diisopropylether and collected by filtration, giving 2.1 g of the title compound (98%).
後処理
- temperatureThe resulting solution was refluxed
- customThe solvent was then evaporated
- dissolutionthe crude was dissolved with dichloromethane
- washwashed with water
- dry with materialThe organic layer was dried over sodium sulphate
- customthe solvent removed in vacuo
- customThe residue was then triturated with diisopropylether
- filtrationcollected by filtration
出典と根拠
- ORDレコード
- ord-dd9a691f4ee84b31a5d3a8965a711945
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541575B2
反応ノート
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