反応式
[CH2:1]([O:3][C:4]([CH:6]=[C:7]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[N:11]([C:19](=[O:37])[C:20]2[CH:25]=[CH:24][C:23]([NH:26][C:27](=[O:35])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[CH3:34])=[CH:22][C:21]=2[CH3:36])[CH2:10][CH2:9][CH2:8]1)=[O:5])[CH3:2].[BH4-].[Na+]>O1CCCC1.CO.O.O.O.O.O.O.[Ni](Cl)Cl>[CH2:1]([O:3][C:4]([CH2:6][CH:7]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[N:11]([C:19](=[O:37])[C:20]2[CH:25]=[CH:24][C:23]([NH:26][C:27](=[O:35])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[CH3:34])=[CH:22][C:21]=2[CH3:36])[CH2:10][CH2:9][CH2:8]1)=[O:5])[CH3:2]参加物
反応物 2
生成物 1
試薬・触媒・溶媒 2
実験手順
5-Ethoxycarbonylmethylidene-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.30 g) and nickel chloride hexahydrate (0.55 g) are dissolved in a mixture of tetrahydrofuran/methanol (1:1) (30 ml), and to the mixture is added slowly sodium borohydride (0.26 g) with stirring under ice-cooling, and then the mixture is further stirred for 10 minutes under ice-cooling. The insoluble materials are filtered with Celite, and the filtrate is concentrated. The resulting residue is purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:1) to give 5-ethoxycarbonylmethyl-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.13 g) as colorless amorphous.
後処理
- temperaturecooling
- stirringthe mixture is further stirred for 10 minutes under ice-
- temperaturecooling
- filtrationThe insoluble materials are filtered with Celite
- concentrationthe filtrate is concentrated
- customThe resulting residue is purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:1)
出典と根拠
- ORDレコード
- ord-be3698e1a0504a98b5ed49a7b8e68b9f
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05244898
関連ノート
読み込み中…