Reaktion #84149
ord-5832e3deb7e74ffd9ceb999f45ff1987
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe solvent was evaporated in vacuo
- 2Sonstigethe residue partitioned between H2O (15 mL) and EtOAc (15 mL)
- 3SonstigeThe layers were separated
- 4Extraktionthe aqueous phase extracted with EtOAc (2×15 mL)
- 5TrocknenThe combined organics were dried (MgSO4)
- 6Filtrationfiltered
- 7Sonstigethe solvent evaporated in vacuo
Vorschrift
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+).