反应详情

温度

130 °C

To 1-fluoro-2-methyl-5-(methyloxy)-4-nitrobenzene (Example 113, step B) (0.5 g, 2.7 mmol) in 25 mL of DMSO was added, 1-(methylsulfonyl)piperazine (0.53 g, 3.24 mmol), and K2CO3 (1.12 g, 8.1 mmol). The mixture was heated to 130° C. for 24 h. The mixture was poured into 500 mL of H2O, filter, washed with H2O, air dried for 15 min, dissolved in DCM, dried (MgSO4), filtered, and rotovaped down to give the title compound of step A (0.87 g, 2.64 mmol, 98%). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.77 (s, 1H), 6.76 (s, 1H), 3.89 (s, 3H), 3.23-3.28 (m, 4H), 3.06-3.11 (m, 4H), 2.93 (s, 3H), 2.20 (s, 3H).

1. filtrationfilter
2. washwashed with H2O, air
3. customdried for 15 min
4. dissolutiondissolved in DCM
5. dry with materialdried (MgSO4)
6. filtrationfiltered