反应详情

1-methyl-1H-indazole-3-carboxylic acid (2.64 g) was mixed with methanol (20 ml) and 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholin-4-ium chloride (4.57 g) and methylamine (40% methanol solution, 2.0 ml) were added thereto at room temperature. After stirring at room temperature for 14 hours, the reaction solution was concentrated under reduced pressure. The residue was diluted with ethyl acetate, and the organic layer was washed with water-saturated brine (1:1) and further saturated brine in this order. The organic layer was dried over anhydrous sodium sulfate and was then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-50:50) to obtain N,1-dimethyl-1H-indazole-3-carboxamide (1.84 g) as a colorless solid.

1. additionwere added
2. customat room temperature
3. concentrationthe reaction solution was concentrated under reduced pressure
4. additionThe residue was diluted with ethyl acetate
5. washthe organic layer was washed with water-saturated brine (1:1) and further saturated brine in this order
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. concentrationwas then concentrated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-50:50)