反应详情

温度

100 °C

A mixture of 1-(3-chloro-benzyl)-7-(2-chloro-ethoxy)-5-fluoro-3-(naphthalene-1-sulfonyl)-1H-indazole (0.075 g, 0.14 mmoles) and methylamine (0.56 mmoles) in DMSO (1 mL) was stirred under nitrogen at 100° C. for 4 hours. Mixture was cooled to room temperature, diluted with water, extracted with EtOAc, washed with water (2×), brine (1×), dried over Na2SO4, and concentrated under vacuum. Compound was purified by flash chromatography using as eluent 5% CH3OH/EtOAc. The purified compound was dissolved in methanol, 1M HCl in ether (0.1 mL, 0.1 mmoles) was added, and compound was dried to afford the title compound as the HCl salt.

1. temperatureMixture was cooled to room temperature
2. extractionextracted with EtOAc
3. washwashed with water (2×), brine (1×)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under vacuum
6. customCompound was purified by flash chromatography
7. dissolutionThe purified compound was dissolved in methanol
8. customcompound was dried