反应详情

Dissolve N-methoxy-N-methyl-6-(trifluoromethyl)pyridine-3-carboxamide (0.685 g, 2.92 mmol) in THF (20 mL). Add methylmagnesium bromide (3.0 M in EtO2, 1.950 mL, 5.850 mmol). Stir the mixture for 16 hours. Pour the reaction mixture into a saturated NaHCO3 aqueous solution (20 mL). Extract with EtOAc (3×20 mL). Wash the combined organic extracts with water (30 mL) and saturated sodium chloride (2×30 mL). Dry the organic extracts over sodium sulfate; filter; collect the filtrate; and concentrate the filtrate under reduced pressure to give the title compound (0.545 g, 98%) as a light yellow solid. 1H NMR (400.43 MHz, d6-DMSO) δ 9.21-9.21 (m, 1H), 8.51-8.49 (m, 1H), 8.03 (d, J=8.2 Hz, 1H), 2.64 (s, 3H).

1. extractionExtract with EtOAc (3×20 mL)
2. washWash the combined organic extracts with water (30 mL) and saturated sodium chloride (2×30 mL)
3. dry with materialDry the organic extracts over sodium sulfate
4. filtrationfilter
5. customcollect the filtrate
6. concentrationand concentrate the filtrate under reduced pressure