反应详情

Ethyl 5-methyl 2-fluoro-6-methyl-4-(p-tolyl)pyridine-3,5-dicarboxylate (14 mg, 0.042 mmol) was dissolved in DCE (1 mL). Cyclohexylamine (9.67 ul, 0.085 mmol) and triethylamine (5.89 ul, 0.042 mmol) were added and the reaction was heated at reflux 18 hours. The mixture was concentrated, diluted with ethyl acetate and brine, extracted with ethyl acetate, dried over sodium sulfate, and concentrated to afford the title compound (20 mg) that was used without further purification: 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 7.08-7.15 (m, 2 H) 6.97-7.07 (m, 2 H) 4.04-4.19 (m, 1 H) 3.75-3.88 (m, 2 H) 3.41 (s, 3 H) 2.43 (s, 3 H) 2.35 (s, 3 H) 1.96-2.17 (m, 2 H) 1.55-1.93 (m, 4 H) 1.36-1.53 (m, 2 H) 1.17-1.37 (m, 2 H) 0.56-0.71 (m, 3 H); LCMS (m/z) ES+=411 (M+1).

1. temperaturethe reaction was heated
2. temperatureat reflux 18 hours
3. concentrationThe mixture was concentrated
4. additiondiluted with ethyl acetate and brine
5. extractionextracted with ethyl acetate
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated