反応式
[C:1]([NH:4][C:5]1[C:6](=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:7](O)=[O:8])(=O)[CH3:2].[NH2:14][N:15]1[C:27](=[O:28])[C:25]2[C:26]3[N:18]([C:19]([O:29][CH3:30])=[CH:20][C:21]=3[CH2:22][CH2:23][CH:24]=2)[C:17]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[CH:16]1.P(Cl)(Cl)Cl.[P].C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH3:30][O:29][C:19]1[N:18]2[C:17]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)=[CH:16][N:15]([N:14]3[C:7](=[O:8])[C:6]4[C:5](=[CH:13][CH:12]=[CH:11][CH:10]=4)[N:4]=[C:1]3[CH3:2])[C:27](=[O:28])[C:25]3=[CH:24][CH2:23][CH2:22][C:21]([CH:20]=1)=[C:26]23参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
0.834 g (4.65 mmol) of acetylanthranilic acid and 1.3 g (4.23 mmol) of 3-amino-9-methoxy-1-phenyl-6,7-dihydro-3H-[1,4]diazepino[6,7,1-hi]indol-4-one are dissolved in 13 ml of CH2Cl2, the mixture is stirred at room temperature and 0.7 g (5 mmol) of phosphorus trichloride is added. The mixture is stirred for 20 h and 0.35 g of phosphorus trichlonrde is added, followed by a fuirther 0.35 g 8 h later. The mixture is cooled, 50 ml of saturated NaHCO3 solution and 100 ml of CH2Cl2 are added and the organic phase is separated out after settling has taken place and washed with water. This solution is dried, evaporated and purified by chromatography in the mixture DM1. 0.33 g of yellow powder is obtained. M.p.=277° C.—Yld 17%.—TLC (DM3): Rf=0.47.
後処理
- stirringThe mixture is stirred for 20 h
- customfollowed by a fuirther 0.35 g 8 h
- temperatureThe mixture is cooled
- customthe organic phase is separated out after settling
- washwashed with water
- customThis solution is dried
- customevaporated
- custompurified by chromatography in the mixture DM1
出典と根拠
- ORDレコード
- ord-f377b519db484db3a2f9106d17541b22
- 出典データセット
- uspto-grants-2001_05
- 特許番号
- US06239130B1
関連ノート
読み込み中…