反応 #2326

反応方程式

product

4-acetylaminopiperidine hydrochloride

4-chloropyridine hydrochloride

sodium hydrogen carbonate

→

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

溶媒

3-methyl 1-butanol

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux temperature for 16 hours
3. 3
   ろ過The cooled mixture was filtered
4. 4
   濃縮the filtrate concentrated in vacuo
5. 5
   その他Purification of the residue by flash chromatography on silica
6. 6
   洗浄eluting with methanol/dichloromethane (1:2 v/v)

実験手順

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)+.

出典