반응 #83987

반응 방정식

6-fluoro-3-(4-piperazinyl)-1H-indazole

NaHCO3

CH3CN

→

tan solid

[4-(6-Fluoro-1H-indazol-3-yl)-1-piperazinyl]acetonitrile

용매

H2O

반응 조건

후처리

1. 1
   온도at reflux under N2 for 18 hours
2. 2
   기타The cooled reaction
3. 3
   추출the aqueous solution was extracted with EtOAc
4. 4
   추출The EtOAc extract
5. 5
   세척was washed with H2O
6. 6
   세척washed with brine
7. 7
   건조dried with MgSO4
8. 8
   농축concentrated

실험 절차

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.

출처