CN1CC[O:5][CH2:4]C1.[CH3:8][C@@H:9]1[NH:15][CH2:14][C:13]2[CH:16]=[CH:17][CH:18]=[C:19]([NH2:20])[C:12]=2[NH:11][CH2:10]1.ClC(OC(Cl)(Cl)Cl)=O>ClCCl>[CH3:8][C@@H:9]1[NH:15][CH2:14][C:13]2[CH:16]=[CH:17][CH:18]=[C:19]3[NH:20][C:4](=[O:5])[N:11]([C:12]=23)[CH2:10]1300 ml of dichloromethane and 22.8 ml of 4-methylmorpholine are added to 12.7 g (0.072 mol) of (S)-3-methyl-2,3,4,5-tetrahydro-(1H)-1,4-benzodiazepin-9-amine. The mixture is then poured into a solution of 9.1 ml (0.0072 mol) of trichloromethyl chloroformate in 340 ml of dichloromethane cooled beforehand with an ice bath. The mixture is left stirring for 10 minutes at 0° C. and then for 20 minutes at room temperature. The solvent is evaporated under vacuum and the residue taken up in 200 ml of water and 34 ml of dioxane. The mixture is heated in a water bath for 45 minutes and then a concentrated aqueous ammonia solution is added. The mixture is left to cool, is sucked dry, is washed with water and is dried under vacuum. There are obtained 11.5 g of product which is recrystallized from boiling water. There are obtained 7.6 g of product which is used as is in the following stage.
読み込み中…
