反应详情

To a stirred solution of 9-3 (2.0 g, 3.6 mMol), HOBT (0.5 g, 3.9 mMol), and 1H-1,2,3-triazole-4-carboxylic acid (0.4 g, 3.9 mMol) in anhydrous DMF (20 mL) was added DIEA (1.2 mL, 7.2 mMol) followed by EDC (0.76 g, 3.9 mMol). The solution was stirred at ambient temperature overnight. The solution was then treated with 2 mL of acetic acid and was heated to 80° C. for 3 hrs. Upon cooling to room temperature, the solution was filtered through a syringe filter and purified on a C18 reverse phase HPLC to give 9-4 as a solid. Mass (M+1) calculated: 631.2789 observed: 631.2778

1. temperaturewas heated to 80° C. for 3 hrs
2. temperatureUpon cooling to room temperature
3. filtrationthe solution was filtered through a syringe
4. filtrationfilter
5. custompurified on a C18 reverse phase HPLC