反应详情

温度

75 °C

To a stirred solution of 4-nitro-1H-pyrazole (27) (1.0 g, 8.9 mmol) in MeCN (15 mL) was added K2CO3 (1.8 g, 13.2 mmol) and 3-bromo-propanol (880 μL, 9.7 mmol). The mixture was stirred at 75° C. for 6 hours. The solvent was evaporated in vacuo and the residue partitioned between H2O (15 mL) and EtOAc (15 mL). The layers were separated and the aqueous phase extracted with EtOAc (2×15 mL). The combined organics were dried (MgSO4), filtered and the solvent evaporated in vacuo to afford the title compound as a pale yellow oil (1.41 g, 93%); LCMS, Rt=1.31 min (MeOH-FA method), m/z 172 (MH+).

1. customThe solvent was evaporated in vacuo
2. customthe residue partitioned between H2O (15 mL) and EtOAc (15 mL)
3. customThe layers were separated
4. extractionthe aqueous phase extracted with EtOAc (2×15 mL)
5. dry with materialThe combined organics were dried (MgSO4)
6. filtrationfiltered
7. customthe solvent evaporated in vacuo