反应详情

A solution of 2,4-dichlorobenzaldehyde (18 mg) and compound 7 (17 mg) in THF (1 mL) was stirred at room temperature for 1 hour and then sodium triacetoxyborohydride (42 mg) was added in one portion. The mixture was stirred at room temperature for another hour and EtOAc (1 mL) was added followed by the addition of saturated aqueous ammonium chloride (1 mL). The aqueous phase was extracted by EtOAc (3×1 mL) and the combined organic extractants was dried, filtered and concentrated in vacuo. The residue was purified by preparative HPLC to afford the title compound 9 as a white solid (15 mg, 80%). LCMS: Rf: 3.605 min, M+H+: 495.

1. extractionThe aqueous phase was extracted by EtOAc (3×1 mL)
2. customthe combined organic extractants was dried
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was purified by preparative HPLC