反应详情

温度

80 °C

In a microwave vial were added tert-butyl(1-(4-(6-chloro-5-nitro-3-phenylpyridin-2-yl)phenyl)cyclobutyl)carbamate (200 mg, 0.417 mmol), methyl 2-(methylamino)acetate hydrochloride (58 mg, 0.417 mmol) and triethylamine (58 μl, 0.417 mmol) in methanol (2 ml). The solution was heated to 80° C. under microwave irradiation for 1 hour. The reaction mixture was concentrated to dryness under reduced pressure and purified by Biotage chromatography (cyclohexane:ethyl acetate, gradient elution from 100:0 to 0:100) to afford the title compound (103 mg, 65%). 1H NMR (500 MHz, CDCl3): 8.29 (1H, s), 7.25-7.38 (7H, m), 7.15-7.23 (2H, m), 5.05 (1H, br s), 4.39 (2H, s), 3.83 (3H, s), 3.11 (3H, s), 2.25-2.65 (4H, m), 2.05-2.20 (1H, m), 1.80-1.95 (1H, m), 1.10-1.50 (9H, br).

1. concentrationThe reaction mixture was concentrated to dryness under reduced pressure
2. custompurified by Biotage chromatography (cyclohexane:ethyl acetate, gradient elution from 100:0 to 0:100)