反应详情

温度

100 °C

To a solution of 2-fluoro-5-methoxybenzaldehyde (450 mg, 2.92 mmol) in DMSO (13 mL) are added 4-chloro-1H-pyrazole (450 mg, 4.39 mmol) and K2CO3 (810 mg, 5.84 mmol) at room temperature. The solution is heated to 100° C. for 1.5 hours. The solution is cooled down and is diluted with H2O (150 mL) and extracted with EtOAc (3×). The combined organic layers are dried with MgSO4 and filtered. The filtrate is concentrated and the residue is purified by silica gel flash column chromatography with 5-25% EtOAc in heptane as the eluent to afford 2-(4-chloro-pyrazol-1-yl)-5-methoxy-benzaldehyde which is used without further purification

1. temperatureThe solution is cooled down
2. extractionextracted with EtOAc (3×)
3. dry with materialThe combined organic layers are dried with MgSO4
4. filtrationfiltered
5. concentrationThe filtrate is concentrated
6. customthe residue is purified by silica gel flash column chromatography with 5-25% EtOAc in heptane as the eluent