反应详情

温度

60 °C

To a stirred solution of 2-chloro-N-methyl-5-nitropyrimidin-4-amine (1.9 g, 10 mmol) in acetic acid (30 mL) was added iron powder (4 g, 71 mmol), and the suspension mixture was heated to 60° C. for 16 hours. The solvent was removed under reduced pressure, and the residue was diluted by brine and ethyl acetate. The solid was filtered off, and the filtrate was extracted with ethyl acetate (50 mL*12). The organic layers were separated, combined, dried over sodium sulfate, filtered and concentrated to give the title compound (1.1 g, 69%). MS (ES+) C5H7ClN4 requires: 159, 161. found: 160, 162 [M+H]+.

1. customThe solvent was removed under reduced pressure
2. additionthe residue was diluted by brine and ethyl acetate
3. filtrationThe solid was filtered off
4. extractionthe filtrate was extracted with ethyl acetate (50 mL*12)
5. customThe organic layers were separated
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated