反应详情

温度

100 °C

A vessel was charged with 5-bromo-1-methyl-1H-indazol-3-amine (250 mg, 1.10 mmol), 2-chloro-N-(2-chloroethyl)-N-methylethanamine hydrochloride (230 mg, 1.21 mmol), H2O (250 μL), K2CO3 (500 mg, 3.63 mmol), and DMF (2.5 mL). The vessel was sealed and heated to 100° C. for 18 h. The reaction was poured into EtOAc and washed with 5% w/v aq LiCl (3×), dried (Na2SO4), filtered, and concentrated. The residue was treated with DCM and purification by flash column chromatography on silica gel (hexanes/ethyl acetate to remove side products; then DCM/MeOH eluent to elute product) provided 5-bromo-1-methyl-3-(4-methylpiperazin-1-yl)-1H-indazole. LCMS-ESI+: calc'd for C13H17BrN4: 309.1, 311.1 (M+H+); Found: 309.2, 311.2 (M+H+).

1. customThe vessel was sealed
2. washwashed with 5% w/v aq LiCl (3×)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. additionThe residue was treated with DCM and purification by flash column chromatography on silica gel (hexanes/ethyl acetate
7. customto remove side products
8. washthen DCM/MeOH eluent to elute product)