反応式
[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[C:4]([NH:6][C:7]1[CH:15]=[CH:14][C:10]([C:11](Cl)=[O:12])=[CH:9][CH:8]=1)=[O:5].C(N(CC)CC)C.[N:27]1[CH:28]=[CH:29][N:30]2[CH2:36][C:35]3[CH:37]=[CH:38][CH:39]=[CH:40][C:34]=3[NH:33][CH2:32][C:31]=12>C(Cl)Cl>[N:27]1[CH:28]=[CH:29][N:30]2[CH2:36][C:35]3[CH:37]=[CH:38][CH:39]=[CH:40][C:34]=3[N:33]([C:11]([C:10]3[CH:14]=[CH:15][C:7]([NH:6][C:4](=[O:5])[C:3]4[CH:16]=[CH:17][CH:18]=[CH:19][C:2]=4[CH3:1])=[CH:8][CH:9]=3)=[O:12])[CH2:32][C:31]=12参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a mixture of 1.37 g (5 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 15 ml of methylene chloride, cooled to 0° C. is added 1.5 ml of triethylamine. After stirring for 3 minutes, 5 mmol of 10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine in 5 ml of methylene chloride is added. The cooling bath is removed and after about 30 minutes a complete solution is obtained. The reaction mixture is allowed to stir at room temperature for 1 hour and the volatiles are concentrated in vacuo. The residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, and brine. The solution is dried with Na2SO4 and the volatiles concentrated in vacuo to give the desired product as a solid.
後処理
- customThe cooling bath is removed and after about 30 minutes a complete solution
- customis obtained
- stirringto stir at room temperature for 1 hour
- concentrationthe volatiles are concentrated in vacuo
- dissolutionThe residue is dissolved in 100 ml of ethyl acetate
- washwashed with water, 2N citric acid, and brine
- dry with materialThe solution is dried with Na2SO4
- concentrationthe volatiles concentrated in vacuo
出典と根拠
- ORDレコード
- ord-a431122163e447568a7b04ac3c9d729f
- 出典データセット
- uspto-grants-1996_05
- 特許番号
- US05516774
関連ノート
読み込み中…