反应详情

Prepared from 1-(4-methoxybenzyl)-3-methyl-1H-pyrazolo[3,4-b]pyridin-4-ol (0.150 g, 0.557 mmol; prepared as in Example 5, Step B) and 1,3-dichloro-2-fluoro-5-nitrobenzene (0.117 g, 0.557 mmol), according to the procedure of Example 13, Step A. The crude product was purified Biotage 40S column eluting with 3:1 hexane/EtOAc then EtOAc to obtain the product (195 mg, 73%) as an off white solid. 1H NMR (CDCl3, 400 MHz) δ 8.37 (s, 1H), 8.29 (d, J=5.5 Hz, 1H), 7.37 (d, J=8.6 Hz, 2H), 6.85 (d, J=9.0 Hz, 2H), 5.93 (d, J=5.5 Hz, 1H), 5.58 (s, 2H), 3.77 (s, 3H), 2.75 (s, 3H). LRMS (esi pos) m/e 460 (M+1).

1. customThe crude product was purified Biotage 40S column
2. washeluting with 3:1 hexane/EtOAc