反应详情

Ethyl 4-(4-bromo-2-fluoroanilino)-6-chloronicotinate was dissolved in CHCl3 and reacted with Me2SO4, followed by triethylamine, AcOH and EtOH as described for example 33, step B. Purification by recrystallisation (EtOAc/Hexane) gave ethyl 4-(4-bromo-2-fluoroanilino)-1-methyl-6-oxo-1,6-dihydro-3-pyridinecarboxylate (77%); m.p. (EtOAc/Hexane) 159-162° C. 1H NMR [400 MHz, CDCl3] δ 9.34 (br s, 1H), 8.22 (s, 1H), 7.36-7.25 (m, 3H), 5.85 (s, 1H), 4.35 (q, J=7.1 Hz, 2H), 3.54 (s, 3H), 1.39 (t, J=7.1 Hz, 3H). LCMS (APCI−) 369 (100%), 367 (100%). Anal. Calcd for C15H14BrFN2O3: C, 48.8; H, 3.8; N, 7.6. Found C, 49.1; H, 3.8; N, 7.4.

1. customPurification
2. customby recrystallisation (EtOAc/Hexane)