反应详情

To a stirred solution of 3-4 (5 g, 13 mMol), HOBT (1.9 g, 14.3 mMol), and glycolic acid (1.2 g, 15.6 mMol) in anhydrous DMF (100 mL) was added EDC (2.7 g, 14.3 mMol). The solution was stirred overnight at ambient temperature. The solution was then treated with 5 mL of glacial acetic acid and was heated to 80° C. in an oil bath for 2 hours. Upon cooling to room temperature, the reaction was diluted with ethyl acetate and washed with NaHCO3 (aq), water, and brine. The organic layer was dried with MgSO4, filtered and concentrated in vacuo to yield 14-1 as a red solid. LC/MS (M+1) calculated: 425.5; observed: 425.6

1. temperaturewas heated to 80° C. in an oil bath for 2 hours
2. temperatureUpon cooling to room temperature
3. washwashed with NaHCO3 (aq), water, and brine
4. dry with materialThe organic layer was dried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo