反应详情

温度

0 °C

3-((3-Iodo-4-nitro-1H-indazol-1-yl)methyl)-1-methylpyridin-2(1H)-one (0.26 g, 0.63 mmol) was added to MeOH (6 mL) and cooled to 0° C. Zinc (0.21 g, 3.2 mmol) was added to the reaction mixture. Saturated aqueous NH4Cl (6 mL) was added drop-wise and the reaction mixture was stirred for 90 minutes at ambient temperature. The reaction was diluted with MeOH (50 mL), stirred for 5 minutes and filtered. The filtrate was diluted with saturated NH4OAc and the MeOH was removed under vacuum. The aqueous mixture was extracted with CHCl3. The organic layer was washed with brine, dried over MgSO4 and concentrated to provide 3-((4-amino-1H-indazol-1-yl)methyl)-1-methylpyridin-2(1H)-one (0.12 g, 71% yield) as a solid.

1. stirringstirred for 5 minutes
2. filtrationfiltered
3. additionThe filtrate was diluted with saturated NH4OAc
4. customthe MeOH was removed under vacuum
5. extractionThe aqueous mixture was extracted with CHCl3
6. washThe organic layer was washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated