反应详情

To a solution of 23 (100 mg, 0.28 mmol), HOBT (49 mg, 0.36 mmol) and EDC (80 mg, 0.41 mmol) in DMF (5 mL) was added 3-oxo-3-(phenylamino)propanoic acid (1) (65 mg, 0.36 mmol). The reaction mixture was stirred for 1 day and was diluted with EtOAc. The resultant solution was washed with water and brine, dried over anhydrous sodium sulfate and concentrated to provide a residue, which was purified by column chromatography (eluents MeOH—CH2Cl2, 2:98, 5:95) to produce a solid material, which after trituration with EtOAc/hexane afforded 5f as a white solid (74 mg, 51% yield). MS (m/z): 519.2 (M+H).

1. washThe resultant solution was washed with water and brine
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationconcentrated
4. customto provide a residue, which
5. customwas purified by column chromatography (eluents MeOH—CH2Cl2, 2:98, 5:95)
6. customto produce a solid material, which after trituration with EtOAc/hexane