반응 #310761

반응 방정식

chloroacetonitrile

6-fluoro-3-(4-piperidyl)-1,2-benzisoxazole hydrochloride

potassium carbonate

Potassium iodide

→

product

수율 64.0%

6-Fluoro-3-(1-cyanomethyl-4-piperidyl)-1,2-benzisoxazole

수율 64.0%

용매

dimethylformamide

water

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred
2. 2
   온도heated under nitrogen at 80°-85° for 2 hrs
3. 3
   기타The solid was collected
4. 4
   기타dried (vacuum oven)
5. 5
   기타Recrystallization from ethanol-water

실험 절차

A mixture of 3.1 g of 6-fluoro-3-(4-piperidyl)-1,2-benzisoxazole hydrochloride, 4.9 g of potassium carbonate and 30 ml of dimethylformamide was stirred at ambient temperature for 5 min. Potassium iodide (0.24 g) was added, followed by 0.76 ml of chloroacetonitrile. The mixture was stirred and heated under nitrogen at 80°-85° for 2 hrs and then poured into 300 ml of water. The solid was collected and dried (vacuum oven). Recrystallization from ethanol-water yielded 2.0 g (64%) of product. An analytical sample was obtained by combining the 2.0 g sample with 0.8 g of another sample and recrystallizing from ethanol-water to give 2.2 g of product, mp, 126°-128°.

출처