반응 #2326

반응 방정식

product

4-acetylaminopiperidine hydrochloride

4-chloropyridine hydrochloride

sodium hydrogen carbonate

→

4-acetylamino-1-(4-pyridyl)piperidine

용매

3-methyl 1-butanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux temperature for 16 hours
3. 3
   여과The cooled mixture was filtered
4. 4
   농축the filtrate concentrated in vacuo
5. 5
   기타Purification of the residue by flash chromatography on silica
6. 6
   세척eluting with methanol/dichloromethane (1:2 v/v)

실험 절차

A mixture of the product from step (ii) (1.79 g), 4-chloropyridine hydrochloride (1.50 g), sodium hydrogen carbonate (2.86 g) in 3-methyl 1-butanol (25 ml) was heated at reflux temperature for 16 hours. The cooled mixture was filtered and the filtrate concentrated in vacuo. Purification of the residue by flash chromatography on silica, eluting with methanol/dichloromethane (1:2 v/v) gave 4-acetylamino-1-(4-pyridyl)piperidine as a foam, 0.69 g: NMR(d6DMSO) δ 8.10(2H,d), 7.80(1H,bd), 6.80(2H,dd), 3.82(3H,m), 2.93(2H,dt), 1.78(3H,s), 1.77(2H,m), 1.33(2H,dq); m/e 220 (M+H)+.

출처