反应详情

To a suspension of 3-bromo-4-nitro-1H-indazole (Preparation B; 8.51 g, 35.2 mmol) in DMF (60 mL) was added 3-(chloromethyl)-1-ethyl-1H-pyrazole hydrochloride (6.37 g, 35.2 mmol) and K2CO3 (14.6 g, 106 mmol). The reaction mixture was stirred for 16 hours. Most of DMF was removed under reduced pressure. The remaining residue was diluted with EtOAc (300 mL) and washed with H2O. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by silica gel chromatography (EtOAc/hexanes 1:5) to provide the product (9.26 g).

1. customMost of DMF was removed under reduced pressure
2. additionThe remaining residue was diluted with EtOAc (300 mL)
3. washwashed with H2O
4. dry with materialThe organic phase was dried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel chromatography (EtOAc/hexanes 1:5)