반응 #1280482

반응 방정식

N,N-Dibenzyl-2-(piperidin-4-yl)ethanamine

4-bromopyridine HBr

DIPEA

→

N,N-Dibenzyl-2-(1-(pyridin-4-yl)piperidin-4-yl)ethanamine

수율 53.0%

용매

n-butanol

반응 조건

후처리

1. 1
   농축the reaction solution was concentrated under reduced pressure
2. 2
   세척washed with water and sat. NaCl solution (in each case 50 ml),
3. 3
   건조dried over sodium sulfate
4. 4
   농축concentrated under reduced pressure
5. 5
   기타After purification by column chromatography (silica gel, 3.5% MeOH in dichloromethane)
6. 6
   기타a white solid was obtained

실험 절차

N,N-Dibenzyl-2-(piperidin-4-yl)ethanamine (2.4 g, 7.79 mmol, 1 eq) and 4-bromopyridine HBr (1.97 g, 10.12 mmol, 1.3 eq) were dissolved in n-butanol (30 ml) and DIPEA (3.3 ml, 19.47 mmol, 2.5 eq) and the mixture was refluxed for 48 h. After monitoring by thin-layer chromatography, the reaction solution was concentrated under reduced pressure and the residue was taken up in dichloromethane (100 ml), washed with water and sat. NaCl solution (in each case 50 ml), dried over sodium sulfate and concentrated under reduced pressure. After purification by column chromatography (silica gel, 3.5% MeOH in dichloromethane), a white solid was obtained. Yield: 53% (1.6 g, 4.15 mmol).

출처