Hydrazine hydrate (1:1) → Ammonia
反応式
[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]参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-acc3963df842493485c6c9e822535ce0
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745630B2
反応ノート
読み込み中…