反应详情

温度

70 °C

Under inert atmosphere, to a solution of 6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridine (0.4 g, 0.94 mmol, see Example 40/Step 1) in anhydrous THF (10 mL) was added SPHOS Pd precatalyst (0.07 g, 0.094 mmol) and LiHMDS (1.0 M solution in Toluene, 1.9 mL, 1.9 mmol) and the contents were heated at 70° C. After 5 h, the reaction mixture was brought back to ambient temperature and quenched with NH4Cl (5 mL). The organic contents were then extracted with EtOAc and the volatiles were then removed under reduced pressure. The residue thus obtained was purified by a flash column chromatography to afford the title compound. H1NMR (CDCl3, 400 MHz): δ 8.38 (s, 1H), 7.29-7.26 (m, 15H), 5.03 (s, 1H), 4.50 (bs, 2H), 3.93 (s, 3H).

1. customwas brought back to ambient temperature
2. customquenched with NH4Cl (5 mL)
3. extractionThe organic contents were then extracted with EtOAc
4. customthe volatiles were then removed under reduced pressure
5. customThe residue thus obtained
6. customwas purified by a flash column chromatography