反应详情

A solution of tert-butyl(1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate (70 mg, 0.144 mmol) and 2,2,2-trifluoroacetohydrazide (7.3 mg, 0.057 mmol) in p-xylene (1 ml) was heated to 150° C. for 30 minutes under microwave irradiation. The resulting reaction mixture was concentrated to dryness under reduced pressure and purified by Biotage silica gel chromatography (gradient 0% to 20% ethyl acetate in n-hexanes) to give the title compound (7 mg, 20%). LCMS (Method D): RT=1.633 min, M+1=564. 1H NMR (500 MHz, CDCl3): 7.96 (1H, s), 7.36-7.27 (7H, m), 7.21-7.17 (2H, m), 5.63 (2H, s), 2.55-2.40 (4H, m), 2.14-1.98 (1H, m), 1.88-1.78 (1H, m), 1.37-1.20 (9H, bs).

1. customThe resulting reaction mixture
2. concentrationwas concentrated to dryness under reduced pressure
3. custompurified by Biotage silica gel chromatography (gradient 0% to 20% ethyl acetate in n-hexanes)