반응 #83976

반응 방정식

4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine

triethylamine

chloroacetyl chloride

→

white crystals

수율 37.1%

1-(2-Chloroacetyl)-4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine

수율 37.1%

용매

dichloromethane

chloroform

chloroform

반응 조건

후처리

1. 1
   세척washed with H2O and brine
2. 2
   기타The solvent was removed
3. 3
   기타the oily product was purified by flash chromatography (SiO2, 50 g; eluted with DCM and 1% CH3OH in DCM)
4. 4
   기타The pure product was obtained as an oil, 4.2 g
5. 5
   기타Crystallization from ethanol

실험 절차

A solution of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (4.4 g, 20 mmol), triethylamine (2.1 g, 21 mmol) in chloroform (50 ml) was added to a solution of chloroacetyl chloride (2.5 g, 22 mmol) in chloroform (100 ml) dropwise at room temperature. The mixture was stirred for 2 hours. The solution was diluted with dichloromethane (DCM, 100 ml) and then washed with H2O and brine. The solvent was removed and the oily product was purified by flash chromatography (SiO2, 50 g; eluted with DCM and 1% CH3OH in DCM). The pure product was obtained as an oil, 4.2 g. Crystallization from ethanol yielded 2.2 g of white crystals, m.p. 101°-102° C.

출처