반응 #322677

반응 방정식

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

K2CO3

2-chloroacetonitrile

→

2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]acetonitrile

용매

acetonitrile

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 24 hours
3. 3
   여과The insolubles were filtered off
4. 4
   세척rinsed with methylene chloride (DCM)
5. 5
   기타During concentration of the solvents on the rotary evaporator, crystals
6. 6
   기타The crystals were collected
7. 7
   기타The product in the mother liquor was further purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, and 1% CHaOH in DCM)
8. 8
   기타The second crop of product thus obtained
9. 9
   기타The sample was recrystallized once more
10. 10
    기타form ethanol, m.p. 130°-132° C.

실험 절차

A mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (11 g, 50 mmol), K2CO3 (8.5 g, 61.6 mmol) and 2-chloroacetonitrile (5.5 g, 73 mmol) in acetonitrile (250 ml) was heated at reflux for 24 hours. The insolubles were filtered off and rinsed with methylene chloride (DCM). During concentration of the solvents on the rotary evaporator, crystals appeared. The crystals were collected and weighed 5.79 g. The product in the mother liquor was further purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, and 1% CHaOH in DCM). The second crop of product thus obtained weighed 5.2 g. The total yield was 10.9 g. The sample was recrystallized once more form ethanol, m.p. 130°-132° C.

출처