反应详情

The crude ketone from step 1 (23.9 g) was stirred in 500 mL methanol and 100 mL water with 8 mL hydrazine hydrate at reflux under nitrogen for 24 hour. The mixture was cooled, concentrated, diluted with ethyl acetate, washed successively with 1N HCl and brine, dried over MgSO4 and concentrated in vacuo. Recrystallization from ethyl acetate-hexane gave 4-(4-fluorophenyl)-3-[4-(methylthio)phenyl]-1H-pyrazole as a pale yellow solid (16.9 g, 90.1%). Elemental analysis Calc'd for C16H13 N2FS: C, 67.58, H, 4.61, N, 9.85, S, 11.28. Found: C, 67.44, H, 4.76, N, 9.69, S, 11.27.

1. temperatureThe mixture was cooled
2. concentrationconcentrated
3. additiondiluted with ethyl acetate
4. washwashed successively with 1N HCl and brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customRecrystallization from ethyl acetate-hexane