反应详情

To a solution of 4-nitro-1H-pyrazole (450 mg, 3.86 mmol) in acetone (15 mL), 3-fluorophenethyl bromide (784 mg, 3.86 mmol), K2CO3 (2.68 g, 19.301 mmol) and tetrabutylammonium bromide (120 mg, 0.38 mmol) was added. The white suspension was stirred at rt for 2 h, then the reaction mixture was diluted with H2O and EtOAc. The org. layer was separated and the aq. layer was extracted with EtOAc (1×). The combined org. layers were dried (MgSO4), filtered and the solvent was removed under reduced pressure. Purification of by FC (EtOAc/hept 3:7) gave 1-(3-fluorophenethyl)-4-nitro-1H-pyrazole as a off-white solid. LC-MS conditions B: tR=0.75 min, [M+H]+=no ionization.

1. customlayer was separated
2. extractionthe aq. layer was extracted with EtOAc (1×)
3. dry with materiallayers were dried (MgSO4)
4. filtrationfiltered
5. customthe solvent was removed under reduced pressure
6. customPurification of by FC (EtOAc/hept 3:7)