反応式
Cl.[CH:2]([NH2:4])=[NH:3].C[O-].[Na+].CN([CH:11]=[C:12]1[C:18](=O)[C:17]2[CH:20]=[CH:21][CH:22]=[CH:23][C:16]=2[N:15]([C:24](=[O:34])[C:25]2[CH:30]=[CH:29][C:28]([N+:31]([O-:33])=[O:32])=[CH:27][CH:26]=2)[CH2:14][CH2:13]1)C>CO>[N+:31]([C:28]1[CH:29]=[CH:30][C:25]([C:24]([N:15]2[C:16]3[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=3[C:18]3[N:3]=[CH:2][N:4]=[CH:11][C:12]=3[CH2:13][CH2:14]2)=[O:34])=[CH:26][CH:27]=1)([O-:33])=[O:32]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 0.152 g (1.89 mmol) of formamidine hydrochloride in 10 ml of methanol under argon is added 0.102 g (1.89 mmol) of sodium methoxide. After stirring 5 min., a solution of 0.46 g (1.26 mmol) of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepine-5-one in 5 ml of methanol is added and the mixture stirred 18 hours. The solvent is removed, dichloromethane added, and the mixture filtered. The solid is washed with dichloromethane. The combined filtrate is concentrated to dryness to give 0.47 g of tan foam. The preceding solid is purified by chromatography on silica gel. The compound is dissolved in ethyl acetate-dichloromethane and applied to the column. The column is then eluted with ethyl acetate to give 0.25 g of product as pale yellow crystals.
後処理
- stirringthe mixture stirred 18 hours
- customThe solvent is removed
- additiondichloromethane added
- filtrationthe mixture filtered
- washThe solid is washed with dichloromethane
- concentrationThe combined filtrate is concentrated to dryness
出典と根拠
- ORDレコード
- ord-1d1d0e69e1944e578258d2915d5e3011
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05869483
関連ノート
読み込み中…