反応式
[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[NH:9][CH:10]=[CH:11][C:5]=2[CH:4]=1>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1参加物
4
実験手順
A suspension of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (21.9 g, 0.1 mol) and 10% palladium/charcoal (1.5 g) in glacial acetic acid (200 ml) is hydrogenated at 50° C. under a hydrogen pressure of 5 bar. After the catalyst has been filtered off the solvent is evaporated in vacuo and the residue is taken up in methylene chloride. After extraction with sodium bicarbonate solution and washing with water, the product is dried over magnesium sulphate, concentrated by evaporation and purified over silica gel with methylene chloride and then with increasing amounts of methanol (up to 10%).
後処理
- customis hydrogenated at 50° C. under a hydrogen
- filtrationAfter the catalyst has been filtered off the solvent
- customis evaporated in vacuo
- extractionAfter extraction with sodium bicarbonate solution
- washwashing with water
- dry with materialthe product is dried over magnesium sulphate
- concentrationconcentrated by evaporation
- custompurified over silica gel with methylene chloride
出典と根拠
- ORDレコード
- ord-04c6be61b72646a7b422c1fdb6bb4583
- 出典データセット
- uspto-grants-1988_04
- 特許番号
- US04737495
関連ノート
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