반응 #83902

반응 방정식

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

cis-1,2-cyclohexanedicarboxylic anhydride

HCl

→

cis-2-[4-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]butyl]hexahydro-1H-isoindole-1,3-dione hydrochloride

용매

pyridine

pyridine

ethanol

ethanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 8 hours
3. 3
   기타was removed to dryness
4. 4
   기타The crude product was purified on a silica gel column
5. 5
   기타The material thus obtained
6. 6
   기타Crystallization
7. 7
   온도upon cooling
8. 8
   기타The crystals were collected

실험 절차

A mixture of 1-(4-aminobutyl)-4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (4.7 g, 16.1 mmol) and cis-1,2-cyclohexanedicarboxylic anhydride (3.23 g, 21 mmol) in pyridine (45 ml) was heated at reflux for 8 hours. At the end of the reaction, pyridine was removed to dryness. The crude product was purified on a silica gel column. The material thus obtained weighed 3.18 g (45%) as a clear oil. This oil was dissolved in ethanol (15 ml), then was treated with HCl in ethanol (45 ml). Crystallization took place upon cooling. The crystals were collected, 3.2 g, m.p.=229°-231° C.

출처