反应详情

0.3 g (0.528 mmol) of (1S)—N-[3-amino-1-(5-chloro-1H-benzimidazol-2-yl)propyl]-3-methyl-4-(pyrrolidin-1-ylcarbonyl)benzamide is suspended in 10 mL of tetrahydrofuran and 0.1 mL (1.056 mmol) of triethylamine and, after the addition of 56 mg (0.528 mmol) of 2-chloroethyl isocyanate, stirred for 16 hours at ambient temperature. Then the solution is concentrated, the residue is taken up in dichloromethane, washed several times with water, and the combined organic extracts are dried and concentrated by evaporation. Yield: 49%; Rf value: 0.30 (silica gel; dichloromethane/ethanol=9:1); C26H30Cl2N6O3 (545.47); mass spectrum: (M+H)+=545/547 (chlorine isotope).

1. concentrationThen the solution is concentrated
2. washwashed several times with water
3. customthe combined organic extracts are dried
4. concentrationconcentrated by evaporation