تفاعل #83986

معادلة التفاعل

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

K2CO3

3-bromopropionitrile

→

nitrile

المردود 31.5%

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

المردود 31.5%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةat reflux for 24 hours
3. 3
   درجة الحرارةThe mixture was cooled
4. 4
   ترشيحthe insolubles were filtered
5. 5
   أخرىThe solvent was removed on a rotary evaporator
6. 6
   أخرىthe crude product was purified by flash chromatography over a silica gel column (SiO2, 120 g)
7. 7
   أخرىThe product thus purified
8. 8
   أخرىRecrystallization from ethanol

الإجراء التجريبي

A mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (11 g, 50 mmol), K2CO3 (8.5 g, 74 mmol) and 3-bromopropionitrile (8.2 g, 1.2 eq) in acetonitrile (300 ml) was heated at reflux for 24 hours. The mixture was cooled and the insolubles were filtered. The solvent was removed on a rotary evaporator and the crude product was purified by flash chromatography over a silica gel column (SiO2, 120 g). The product thus purified weighed 8.94 g. Recrystallization from ethanol yielded the nitrile as white crystals 4.3 g, m.p. 100°-101° C.

المصدر