반응 #83963

반응 방정식

3-piperazin-1-yl-1H-indazole

NaHCO3

chloroacetonitrile

→

product

수율 55.8%

[4-(1H-Indazol-3-yl)-1-piperazinyl]acetonitrile

수율 55.8%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도The suspension was warmed
2. 2
   온도to reflux for 17.5 hours
3. 3
   여과subsequently filtered
4. 4
   세척The remaining solids were washed with dichloromethane
5. 5
   농축the combined filtrates were concentrated
6. 6
   기타The resulting brown oil was purified via flash column chromatography (silica gel, 0-50% EtOAc/DCM)

실험 절차

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.

출처