反応式
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:9][OH:10].Cl.[OH-].[Na+]>C(O)C.O>[CH:1](=[N:9]/[OH:10])/[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
6
実験手順
To a stirred solution of benzaldehyde (3 g, 28.3 mmol) in ethanol (50 mL) and water (30 mL), NH2OH hydrochloride (3.9 g, 56.6 mmol) and sodium hydroxide (2.26 g, 56.6 mmol) were added. The mixture was heated at reflux for 6 hours. The resulting mixture was cooled to room temperature and extracted with EtOAc, and the organic layer was dried over anhydrous sodium sulfate. The solution was then concentrated under vacuum to give the title compound as an oil-like solid (3.4 g), which was used in the next step without further purification. MS (ESI) m/z 121 (M+H+).
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 6 hours
- extractionextracted with EtOAc
- dry with materialthe organic layer was dried over anhydrous sodium sulfate
- concentrationThe solution was then concentrated under vacuum
出典と根拠
- ORDレコード
- ord-f19df7ebeba944b88fc980f07852d648
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969349B2
関連ノート
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