反应详情

温度

80 °C

To a stirred solution of 16-2 (0.08 g, 0.2 mMol), HOBT (0.03 g, 0.2 mMol), and isonicotinic acid (0.02 g, 0.2 mMol) in anhydrous DMF (1 mL) was added DIEA (0.08 mL, 0.5 mMol) followed by EDC (0.04 g, 0.2 mMol). The solution was heated in a microwave reactor at 80° C. for 12 min. The solution was then treated with 0.5 mL of acetic acid and was heated in a microwave reactor at 80° C. for 30 minutes. Upon cooling to room temperature, the volatiles were evaporated in vacuo and the solution was filtered through a syringe filter and purified on a C18 reverse phase HPLC to give 16-3 as a solid. Mass (M+1) calculated: 429.1822 observed: 429.1811

1. temperaturewas heated in a microwave reactor at 80° C. for 30 minutes
2. temperatureUpon cooling to room temperature
3. customthe volatiles were evaporated in vacuo
4. filtrationthe solution was filtered through a syringe
5. filtrationfilter
6. custompurified on a C18 reverse phase HPLC