反应详情

温度

23.5 °C

4-Amino-chroman-7-carbonitrile (Step E) (50 mg, 0.28 mmol), 3-(naphthalen-2-ylsulfonylamino)-3-phenyl-propionic acid (100 mg, 0.28 mmol), HOBt (42 mg, 0.31 mmol), and DIEA (72 mg, 0.56 mmol) were dissolved in CH2Cl2 (10 mL). EDC (52 mg, 0.34 mmol) was added and the reaction was stirred at 22-25° C. overnight until completed. The reaction solution was washed with dilute (˜5%) NaHCO3—H2O and H2O, and solution was dried over MgSO4, filtered and concentrated in vacuo to provide a residue which was purified by column chromatography (silica gel, 25% hexane in EtOAc) to provide the title compound as a white solid mixture of diastereomers (ca. 3:2 by 1H NMR after flash column chromotography).

1. washThe reaction solution was washed
2. additionwith dilute (˜5%) NaHCO3—H2O and H2O, and solution
3. dry with materialwas dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto provide a residue which
7. customwas purified by column chromatography (silica gel, 25% hexane in EtOAc)
8. customto provide