反应详情

The crude 5-amino-1-(2-fluoro-4-methoxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile (256 mg, 1.04 mmol) from above was dissolved in CH2Cl2 (25 mL) and BBr3 (1 M solution in DCM, 5 mL, 5.0 mmol) was added and stirred over night. CH2Cl2 and water were added and the phases separated. The aqueous phase was again extracted with EtOAc/CH2Cl2 (1:1). The solution was dried using a phase separator and concentrated under reduced pressure to give 5-amino-1-(2-fluoro-4-hydroxyphenyl)-3-methyl-1H-pyrazole-4-carbonitrile (217 mg, 76%), which was used as such in the next step.

1. customthe phases separated
2. extractionThe aqueous phase was again extracted with EtOAc/CH2Cl2 (1:1)
3. customThe solution was dried
4. concentrationconcentrated under reduced pressure