反应详情

To a stirred suspension of 4-(6-fluoro-1H-indazol-3-yl)piperidine (4.95 g, 22.6 mmol) and NaHCO3 (2.1 g, 24.9 mmol) in dry acetonitrile (110 ml) was added chloroacetonitrile (1.6 ml, 24.9 mmol) at room temperature, under nitrogen. The suspension was warmed to reflux for 22.5 hours, cooled to room temperature, and subsequently filtered. The remaining solids were washed with DCM and the combined filtrates were concentrated. The resulting brown oil was dissolved into EtOAc and washed with water. The organic phase was dried (MgSO4), filtered and concentrated to give a brown solid which was re-dissolved into DCM/EtOAc and flushed through alumina with DCM. The eluent was concentrated to give 5.2 g of the desired product as a solid, m.p. 149°-151 ° C.

1. temperatureThe suspension was warmed
2. temperatureto reflux for 22.5 hours
3. filtrationsubsequently filtered
4. washThe remaining solids were washed with DCM
5. concentrationthe combined filtrates were concentrated
6. dissolutionThe resulting brown oil was dissolved into EtOAc
7. washwashed with water
8. dry with materialThe organic phase was dried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customto give a brown solid which
12. customflushed through alumina with DCM
13. concentrationThe eluent was concentrated