反应详情

A mixture of 6-fluoro-3-(4-piperazinyl)-1H-indazole (6.0 g, 2.7 mmol), NaHCO3 (2.5 g, 3.0 mmol) chloroacetonitrile (2.5 g, 3.3 mmol) and CH3CN (150 mol) was stirred at reflux under N2 for 18 hours. The cooled reaction was poured into H2O and the aqueous solution was extracted with EtOAc. The EtOAc extract was washed with H2O, washed with brine, dried with MgSO4 and concentrated to yield 7.0 g of a tan solid. A 1.3 g sample was recrystallized from EtOAc to yield 0.65 g of a beige solid, m.p. 154°-156° C.

1. temperatureat reflux under N2 for 18 hours
2. customThe cooled reaction
3. extractionthe aqueous solution was extracted with EtOAc
4. extractionThe EtOAc extract
5. washwas washed with H2O
6. washwashed with brine
7. dry with materialdried with MgSO4
8. concentrationconcentrated