反应详情

Treat a solution of 3-(4-fluorophenyl)pyrazole (7.17 g, 44.2 mmol) in dry DMF (60 mL) with NaH (2.2 g, 92.8 mmol) at 0° C. for 15 min. Add iodomethane (3.3 mL, 53.04 mmol) and slowly warm to RT. Quench the reaction mixture with methanol (5 mL) and dilute with water (100 mL). Extract with EtOAc (3×70 mL), dry (MgSO4) and concentrate and purify (Biotage system eluting with dichloromethane:methanol 50:1) to give desired compound as a white solid (2.3 g, 29% yield).

1. customQuench the reaction mixture with methanol (5 mL)
2. additiondilute with water (100 mL)
3. extractionExtract with EtOAc (3×70 mL)
4. dry with materialdry (MgSO4)
5. concentrationconcentrate
6. custompurify
7. wash(Biotage system eluting with dichloromethane:methanol 50:1)