反应详情

To (5-(benzyloxy)-6-methylpyridin-2-yl)methanol (3.51 g, 15.3 mmol, Prepared as described in U.S. Pat. No. 3,952,101) in DCM (10 mL) was added sulfurous dichloride (10.9 g, 91.9 mmol). The reaction mixture was stirred for 3 hours, and then solvent was removed under reduced pressure. To the resulting solid was added 3-bromo-4-nitro-1H-indazole (3.71 g, 15.3 mmol), K2CO3 (6.35 g, 45.9 mmol) and anhydrous DMF (20 mL). The reaction mixture was stirred for 18 hours. The solvent was removed under reduced pressure. The residue was diluted with water (50 mL) and extracted with EtOAc. The combined organic extracts were dried (Na2SO4), and concentrated, and the residue was purified by silica gel flash chromatography (1:3 EtOAc/hexanes) to give desired product (87%).

1. customsolvent was removed under reduced pressure
2. stirringThe reaction mixture was stirred for 18 hours
3. customThe solvent was removed under reduced pressure
4. additionThe residue was diluted with water (50 mL)
5. extractionextracted with EtOAc
6. dry with materialThe combined organic extracts were dried (Na2SO4)
7. concentrationconcentrated
8. customthe residue was purified by silica gel flash chromatography (1:3 EtOAc/hexanes)