反应详情

温度

60 °C

A mixture of 3-methyl-2-pyridylhydrazine (1.0 g, 8.13 mmol), acetic acid (7.0 mL) and ethyl trifluoroacetoacetate (1.2 mL, 8.13 mmol) was heated at 60° C. for 9 hours. The reaction mixture was neutralized with NaHCO3 and then was extracted with EtOAc (3×). The EtOAc extracts were combined, dried over MgSO4, filtered and concentrated to afford crude product which was purified by column chromatography on silica gel to afford 200 mg of 1-(3-methyl-2-pyridyl)-3-trifluoromethyl-5-hydroxypyrazole.

1. extractionwas extracted with EtOAc (3×)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customto afford crude product which
6. customwas purified by column chromatography on silica gel