反应详情

Sec-butyl-[4-(chloro-4-difluoromethoxy-phenyl)-3-nitro-2,3-dihydro-pyridin-2-yl]-amine (0.145 g, 0.43 mmol) was dissolved in toluene (20 mL), followed by methyl pyruvate (77 μL, 0.86 mmol) and heated to reflux overnight. The reaction was concentrated in vacuo and purified by reverse phase prep HPLC giving 4-sec-butyl-8-(2-chloro-4-difluoromethoxy-phenyl)-2-methyl-4H-pyrido[2,3-b]pyrazin-3-one (Example 113): 1H NMR (300 MHz, CDCl3) δ 8.53–8.52 (d, 1H, J=4.8 Hz), 7.35–7.32 (m, 2H), 7.19–7.13 (m, 2H), 6.85–6.36 (t, 1H, J=73.2 Hz), 2.47 (s, 3H), 2.40–2.20 (m, 1H), 2.10–2.07 (m,1H), 1.65–1.63 (d, 3H, J=6.9 Hz), 0.89–0.84 (t, 3H, J=3.7). MS(AP) m/z 394.2 [(M+H)+, 100], 435.3 [(M+H+CH3CN)+, 10].

1. temperatureheated
2. temperatureto reflux overnight
3. concentrationThe reaction was concentrated in vacuo
4. custompurified by reverse phase prep