Water → 7-Phenyl-1,2-diazapin-3-one
反応式
[C:1]([CH2:9][CH2:10][CH2:11][C:12]([OH:14])=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:16][NH2:17]>C1(C)C=CC=CC=1.CCOCC>[C:2]1([C:1]2[N:17]=[N:16][C:12](=[O:14])[CH:11]=[CH:10][CH:9]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
6
実験手順
To a mixture of 10 g (0.052 mole) of 4-benzoylbutyric acid in 300 ml of toluene, hydrazine was added in one portion and the reaction was heated to reflux until all water had ceased to azeotrope. The reaction mixture was cooled and the toluene was stripped off in vacuo. The residue was dissolved in 200 ml Et2O and washed with H2O (100 ml) and brine (100 ml). The ether extract was dried over anhydrous MgSO4, filtered and stripped to yield an orange semisolid which was triturated with ether to yield 3.8 g (39%) of the desired product as a yellow solid.
後処理
- additionwas added in one portion
- temperaturethe reaction was heated
- temperatureThe reaction mixture was cooled
- washwashed with H2O (100 ml) and brine (100 ml)
- extractionThe ether extract
- dry with materialwas dried over anhydrous MgSO4
- filtrationfiltered
- customto yield an orange semisolid which
- customwas triturated with ether
出典と根拠
- ORDレコード
- ord-e87aace35dd246b89ebaa26756e4c33e
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728694
反応ノート
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