반응 #327596

반응 방정식

2-(pyrimidin-4-yl)nicotinic acid dihydrochloride

4-(2,4-difluorobenzyl)-4-hydroxypiperidine hydrochloride

HATU

triethylamine

→

title compound

수율 33.4%

(4-(2,4-difluorobenzyl)-4-hydroxypiperidin-1-yl)(2-(pyrimidin-4-yl)pyridin-3-yl)methanone

수율 33.4%

용매

water

DMF

반응 조건

후처리

1. 1
   추출the mixture was extracted with ethyl acetate
2. 2
   세척The extract was washed with saturated brine
3. 3
   건조dried over anhydrous sodium sulfate
4. 4
   기타The solvent was evaporated under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)
6. 6
   기타recrystallized from ethyl acetate/hexane

실험 절차

A suspension of 2-(pyrimidin-4-yl)nicotinic acid dihydrochloride (0.36 g), 4-(2,4-difluorobenzyl)-4-hydroxypiperidine hydrochloride (0.42 g), HATU (0.75 g) and triethylamine (1.1 mL) in DMF (5 mL) was stirred overnight at room temperature. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane), and recrystallized from ethyl acetate/hexane to give the title compound (0.18 g).

출처