تفاعل #83985

معادلة التفاعل

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

K2CO3

2-chloroacetonitrile

→

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

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةat reflux for 24 hours
3. 3
   ترشيحThe insolubles were filtered off
4. 4
   غسيلrinsed with methylene chloride (DCM)
5. 5
   أخرىDuring concentration of the solvents on the rotary evaporator, crystals
6. 6
   أخرىThe crystals were collected
7. 7
   أخرىThe product in the mother liquor was further purified by flash chromatography over a silica gel column (SiO2, 70 g; eluted with DCM, and 1% CH3OH in DCM)
8. 8
   أخرىThe second crop of product thus obtained
9. 9
   أخرىThe sample was recrystallized once more form ethanol, m.p. 130°-132° C.

الإجراء التجريبي

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% CH3OH 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.

المصدر