反应详情

A mixture of tert-butyl(2S,4S)-4-(methoxymethyl)-2-(5-{2-[(2S,5S)-5-methylpyrrolidin-2-yl]-1,11-dihydroisochromeno[4′,3′:6,7]naphtho[1,2-d]imidazol-9-yl}-1H-imidazol-2-yl)pyrrolidine-1-carboxylate (101 mg, 0.159 mmol), (2S,3R)-3-methoxy-2-(methoxycarbonylamino)butanoic acid (30 mg, 0.159 mmol), HATU (61 mg, 0.159 mmol) and 2 mL 10% DIPEA in DMF was stirred at room temperature for 1.5 hours. Saturated sodium bicarbonate was added and the product was extracted into dichloromethane, dried over sodium sulphate, filtered and concentrated under reduced pressure. This crude product was treated with 5 mL 1.25N HCl in ethanol at 50° C. for 4 h and then it was concentrated under reduced pressure. Saturated sodium bicarbonate was added and the product was extracted into dichloromethane, dried over sodium sulphate, filtered and concentrated under reduced pressure. (74.6 mg)

1. extractionthe product was extracted into dichloromethane
2. dry with materialdried over sodium sulphate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. additionThis crude product was treated with 5 mL 1.25N HCl in ethanol at 50° C. for 4 h
6. concentrationit was concentrated under reduced pressure
7. additionSaturated sodium bicarbonate was added
8. extractionthe product was extracted into dichloromethane
9. dry with materialdried over sodium sulphate
10. filtrationfiltered
11. concentrationconcentrated under reduced pressure