反应详情

温度

80 °C

3-Aminobenzamide (54 mg, 0.39 mmol) was added to a solution of thiocarbonyldiimidazole (71 mg, 0.39 mmol) in CH3CN (5 mL) and the mixture was stirred for 16 h. Methyl [trans-4-(4-{[hydrazino(oxo)acetyl]amino}phenyl)cyclohexyl]acetate (Intermediate 43) (110 mg, 0.33 mmol) and DMF (5 mL) was added and the mixture was stirred at 50° C. until a clear solution was obtained. PS-CDI (527 mg) was added and the temperature raised to 80° C. for 16 h. The mixture was filtered whilst hot and the polymer washed with DMF (2×5 mL). The filtrates were concentrated by evaporation to give the title compound as a solid; MS m/e (M+Na)+ 500; HPLC retention time=2.26 minutes.

1. stirringthe mixture was stirred at 50° C. until a clear solution
2. customwas obtained
3. filtrationThe mixture was filtered whilst hot and the polymer
4. washwashed with DMF (2×5 mL)
5. concentrationThe filtrates were concentrated by evaporation