反应详情

To a stirred suspension of 3-piperazin-1-yl-1H-indazole (6.0 g, 29.7 mmol) and NaHCO3 (2.7 g, 32.7 mmol) in dry acetonitrile (125 ml) was added chloroacetonitrile (2.1 ml, 31.2 mmol) at room temperature, under nitrogen. The suspension was warmed to reflux for 17.5 hours, cooled to room temperature, and subsequently filtered. The remaining solids were washed with dichloromethane and the combined filtrates were concentrated. The resulting brown oil was purified via flash column chromatography (silica gel, 0-50% EtOAc/DCM) to give 4.0 g of product as an off-white solid, m.p. 121°-123° C.

1. temperatureThe suspension was warmed
2. temperatureto reflux for 17.5 hours
3. filtrationsubsequently filtered
4. washThe remaining solids were washed with dichloromethane
5. concentrationthe combined filtrates were concentrated
6. customThe resulting brown oil was purified via flash column chromatography (silica gel, 0-50% EtOAc/DCM)