反应详情

3-Bromo-4-nitro-1H-indazole (Preparation B; 0.49 g, 2.04 mmol) was dissolved in dimethyl formamide (5 mL). Potassium carbonate (1.13 g, 8.15 mmol) was added followed by 3-(bromomethyl)-1-methylpyridin-2(1H)-one (0.41 g, 2.04 mmol). The mixture was stirred at ambient temperature for two days. The mixture was diluted with ethyl acetate (8 mL) and concentrated under vacuum to give a dark solid which was dried overnight under high vacuum. This material was dissolved in ethyl acetate (80 mL) and washed with water (40 mL). The aqueous layer was extracted twice with ethyl acetate. The combined organic extracts were dried over sodium sulfate and concentrated under vacuum to give a green solid. This material was triturated with diethyl ether and the solids were collected by filtration and dried under high vacuum to give 3-((3-bromo-4-nitro-1H-indazol-1-yl)methyl)-1-methylpyridin-2(1H)-one as a beige solid (552 mg).

1. concentrationconcentrated under vacuum
2. customto give a dark solid which
3. customwas dried overnight under high vacuum
4. dissolutionThis material was dissolved in ethyl acetate (80 mL)
5. washwashed with water (40 mL)
6. extractionThe aqueous layer was extracted twice with ethyl acetate
7. dry with materialThe combined organic extracts were dried over sodium sulfate
8. concentrationconcentrated under vacuum
9. customto give a green solid
10. customThis material was triturated with diethyl ether
11. filtrationthe solids were collected by filtration
12. customdried under high vacuum