تفاعل #2326

معادلة التفاعل

product

4-acetylaminopiperidine hydrochloride

4-chloropyridine hydrochloride

sodium hydrogen carbonate

→

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

المذيبات

3-methyl 1-butanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةat reflux temperature for 16 hours
3. 3
   ترشيحThe cooled mixture was filtered
4. 4
   تركيزthe filtrate concentrated in vacuo
5. 5
   أخرىPurification of the residue by flash chromatography on silica
6. 6
   غسيلeluting with methanol/dichloromethane (1:2 v/v)

الإجراء التجريبي

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)+.

المصدر