反应详情

3-Ethyl 5-methyl 2-fluoro-6-methyl-4-(p-tolyl)pyridine-3,5-dicarboxylate (500 mg, 1.51 mmol) (Example 73, Step A), 2-methoxyethanamine (5 eq., 7.55 mmol, 0.65 mL), DIPEA (2 eq. 3.02 mmol, 0.53 mL) and DCE (5 mL) were combined and heated in a microwave reactor set at 140° C. for 1 hour. The mixture was diluted with saturated sodium bicarbonate solution, extracted with DCM, dried over sodium sulfate and purified by silica-gel chromatography to give the title compound to Step A (285 mg, 49%). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm=7.49 (m, 1 H), 7.12 (m, 2 H), 7.03 (m, 2 H), 3.85 (m, 2 H), 3.74 (m, 2 H), 3.60 (m, 2 H), 3.44-3.40 (m, 6 H), 2.44 (s, 3 H), 2.35 (s, 3 H), 0.67 (m, 3 H); LCMS (m/z) ES+=387.33 (M+1).

1. temperatureheated in a microwave reactor
2. extractionextracted with DCM
3. dry with materialdried over sodium sulfate
4. custompurified by silica-gel chromatography