CO.Cl([O-])(=O)(=O)=O.[CH2:8]([C:10]1([C:27]#[N:28])[C:19]2[NH+:14]([CH2:15][CH2:16][C:17]3[C:18]=2[N:20]=[C:21]2[C:26]=3[CH:25]=[CH:24][CH:23]=[CH:22]2)[CH2:13][CH2:12][CH2:11]1)[CH3:9].[B-].[Na+]>C(Cl)Cl>[CH2:8]([C:10]1([C:27]#[N:28])[CH:19]2[N:14]([CH2:15][CH2:16][C:17]3[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[NH:20][C:18]=32)[CH2:13][CH2:12][CH2:11]1)[CH3:9]In a 1-liter round-bottomed flask there were placed 200 ml methanol, 100 ml methylene chloride and 13.5 g (0.036 mole) of the perchlorate of step (c) above. The flask was cooled to about 5° C. and 5 g of sodium borohydrate were added in small quantities. The solution was then stirred for 2 hours at room temperature, concentrated, washed with water and extracted with methylene chloride. After drying and removing the solvent, there were obtained 8 g of yellow crystals, recrystallized from isopropyl ether, melted at 160° C. (yield 80%). The results of analysis are as follows:
読み込み中…
