تفاعل #83976

معادلة التفاعل

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

triethylamine

chloroacetyl chloride

→

white crystals

المردود 37.1%

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

المردود 37.1%

المذيبات

dichloromethane

chloroform

chloroform

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر