反应详情

1-(2-fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine (10 g, 38 mmol) and potassium tert. butoxide (5 g, 46 mmol) was stirred under argon atmosphere in NMP (50 mL) at 150° C. for 45 min. The reaction mixture was then cooled and poured with stirring into ice-water and extracted trice with ethyl acetate. The combined organic phases were washed with water and brine, and were then evaporated. The residue crystallized slowly from methanol-water to afford 1-(4-fluorophenyl)-5-methoxy-1H-indazole as beige crystals (3.32 g, 36%)

1. temperatureThe reaction mixture was then cooled
2. additionpoured
3. extractionextracted trice with ethyl acetate
4. washThe combined organic phases were washed with water and brine
5. customwere then evaporated
6. customThe residue crystallized slowly from methanol-water