反应详情

To a suspension of N-(4-(benzyloxy)pyridin-3-yl)methanesulfonamide (30 g, 0.11 mol) and K2CO3 (14.9 g, 0.11 mol) in DMF (300 mL) was added dropwise CH3I (15.3 g, 0.11 mol) at 0° C. under N2, and then the mixture was stirred for 1 hour at this temperature. H2O was added to the mixture and extracted with dichloromethane. The combined organic layer was washed with H2O, brine, dried over Na2SO4, filtrated and concentrated in vacuo to give N-(4-(benzyloxy)pyridin-3-yl)-N-methylmethanesulfonamide (15 g, yield: 50%), which was used for the next step without further purification. 1H-NMR (CDCl3, 400 MHz) δ 8.46 (s, 1H), 8.41 (d, J=6.0 Hz, 1H), 7.37˜7.39 (m, 5H), 6.94 (d, J=6.0 Hz, 1H), 5.15 (s, 2H), 3.22 (s, 3H), 2.79 (s, 3H). MS (M+H)+: 293.

1. extractionextracted with dichloromethane
2. washThe combined organic layer was washed with H2O, brine
3. dry with materialdried over Na2SO4
4. filtrationfiltrated
5. concentrationconcentrated in vacuo