反应详情

A solution of 3-ethyl 5-methyl 2-amino-6-methyl-4-(p-tolyl)-1,4-dihydropyridine-3,5-dicarboxylate (2 g, 6.05 mmol) in dichloromethane (DCM) (30 ml) was treated with DDQ (1.374 g, 6.05 mmol) and stirred at rt for 1.5 hours. The reaction was filtered through a pad of celite and washed with DCM. The filtrate was diluted with sat. NaHCO3, extracted with DCM, washed with brine, dried with Na2SO4, filtered, and concentrated to afford 3-ethyl 5-methyl 2-amino-6-methyl-4-(p-tolyl)pyridine-3,5-dicarboxylate (1.9145 g, 5.83 mmol, 96% yield) as brown solid: 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 7.14 (d, J=7.8 Hz, 2 H), 7.08-7.00 (m, 2 H), 6.05 (br. s., 2 H), 3.86 (q, J=7.2 Hz, 2 H), 3.45 (s, 3 H), 2.43 (s, 3 H), 2.37 (s, 3 H), 0.69 (t, J=7.2 Hz, 3 H); LCMS (m/z) ES+=329 (M+1).

1. filtrationThe reaction was filtered through a pad of celite
2. washwashed with DCM
3. additionThe filtrate was diluted with sat. NaHCO3
4. extractionextracted with DCM
5. washwashed with brine
6. dry with materialdried with Na2SO4
7. filtrationfiltered
8. concentrationconcentrated