反应详情

A flask equipped with an overhead stirrer and condenser was charged with 1-((6-isopropylpyridin-2-yl)methyl)-3-methyl-4-nitro-1H-indazole (25 g, 0.081 mol) and 150 mL of ethanol, followed by 45 g (0.805 mol) of iron powder. An equal amount of saturated ammonium chloride solution was added and the mixture was brought to 80° C. After 5 hours of heating, the mixture was allowed to cool to ambient temperature, diluted with water (500 mL) and filtered through GF/F filter paper multiple times to remove the iron and iron salts. The filtrate was extracted with EtOAc, dried over sodium sulfate and concentrated under reduced pressure. Column chromatography (1:1 ethyl acetate/hexane to 100% ethyl acetate) afforded 12.6 g (56%) of 1-((6-isopropylpyridin-2-yl)methyl)-3-methyl-1H-indazol-4-amine.

1. customA flask equipped with an overhead stirrer and condenser
2. customwas brought to 80° C
3. temperatureAfter 5 hours of heating
4. filtrationfiltered through GF/F
5. filtrationfilter paper multiple times
6. customto remove the iron and iron salts
7. extractionThe filtrate was extracted with EtOAc
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated under reduced pressure