反应详情

温度

0 °C

To a mixture of N-(2-methyl-2-hydroxyethyl)-N′-cyano-N″-4-pyridylguanidine (0.5 g, 2.2 mmol) and triphenylphosphine (1.2 g, 4.5 mmol) in THF (20 mL) at 0° C. under nitrogen was added diisopropyl azodicarboxylate (0.92 g, 4.5 mmol) dissolved in THF (10 mL) dropwise over 15 minutes. The resulting mixture was stirred at 0° C. for another 2 hours and then warmed to room temperature for 60 hours. After the reaction was complete, the mixture was concentrated and purified by chromatography on silica gel using ethyl acetate as eluant to remove triphenylphosphine and triphenylphosphine oxide followed by clution with a mixture of dichloromethane and methanol (7:1) to afford the product (i.e., Compound 12) as a white solid (0.23 g, 50%).

1. temperaturewarmed to room temperature for 60 hours
2. concentrationthe mixture was concentrated
3. custompurified by chromatography on silica gel
4. customto remove triphenylphosphine and triphenylphosphine oxide
5. additionfollowed by clution with a mixture of dichloromethane and methanol (7:1)