反应详情

(R)-tert-Butyl 4-(tert-butoxycarbonylamino)-7-(2,2-dichloro-N-(2-(3-(2,6-dichlorophenyl)isoxazol-5-yl)pyridin-4-yl)acetamido)-5-oxoheptanoate (165 mg) was dissolved in anhydrous dichloromethane (2 mL) and cooled in an ice-bath under nitrogen. Then trifluoroacetic acid (2 mL) was added. After 4.5 h at 4° C. the mixture was concentrated under reduced pressure. The residue was dissolved and concentrated under reduced pressure again to give (R)-4-amino-7-(2,2-dichloro-N-(2-(3-(2,6-dichlorophenyl)isoxazol-5-yl)pyridin-4-yl)acetamido)-5-oxoheptanoic acid trifluoroacetate salt as a tan solid. 1H NMR (CD3CN): 8.73 (m, 1H), 7.99 (m, 2H), 7.48 (m, 3H), 7.11 (s, 1H), 6.48 (s, 1H), 4.05 (m, 2H), 3.05-2.85 (m, 2H), 2.30 (m, 2H), 2.15 (m, 1H), 1.97 (m, 2H), 1.80 ppm (m, 1H). MW=594 confirmed by LC-MS, tr=10.07 min (Method Y) MH+=592-596.

1. temperaturecooled in an ice-bath under nitrogen
2. concentrationAfter 4.5 h at 4° C. the mixture was concentrated under reduced pressure
3. dissolutionThe residue was dissolved
4. concentrationconcentrated under reduced pressure again