反应详情

温度

50 °C

Ethane, 1-bromo-2-methoxy (5.7 mL, 0.1 mmol) was added to a mixture of (R)-3-{N-(5′-chloro-2′-fluorobiphenyl-4-ylmethyl)-N′-[3-(2-fluorophenyl)isoxazole-5-carbonyl]hydrazino}-2-hydroxypropionic acid (20.0 mg, 38 μmol) and Et3N (13.2 μL, 0.1 mmol) in acetone (1.0 mL, 14 mmol), and resulting mixture was stirred at 50° C. overnight. The mixture was concentrated, and the residue was dissolved in AcOH (1.5 mL), filtered, and purified by reverse phase preparative HPLC to yield the title compound (10.7 mg, purity 95.7%) as a TFA salt. MS m/z [M+H]+ calc'd for C29H26ClF2N3O6, 586.15. found 585.8.

1. customresulting mixture
2. concentrationThe mixture was concentrated
3. dissolutionthe residue was dissolved in AcOH (1.5 mL)
4. filtrationfiltered
5. custompurified by reverse phase preparative HPLC