반응 #70911

반응 방정식

water

N-[(1S)-1-(4-bromophenyl)ethyl]cyclopropanecarboxamide

2,6-bis(trifluoromethyl)-4-[3-(trifluoromethyl)pyrrolidin-3-yl]pyridine

sodium tert-butoxide

→

N-[(1S)-1-(4-{3-[2,6-bis(trifluoromethyl)pyridin-4-yl]-3-(trifluoromethyl)pyrrolidin-1-yl}phenyl)ethyl]cyclopropanecarboxamide

수율 100.9%

용매

toluene

반응 조건

후처리

1. 1
   기타The vessel was sealed
2. 2
   기타at 120° C.
3. 3
   기타for 10 min
4. 4
   추출was then extracted twice with ethyl acetate
5. 5
   세척which was then washed with water
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   여과After the drying agent was filtered off
8. 8
   workup.DISTILLATIONthe solvent was distilled away under the reduced pressure
9. 9
   기타the residue was then purified by silica gel chromatography

실험 절차

To the solution of N-[(1S)-1-(4-bromophenyl)ethyl]cyclopropanecarboxamide (0.134 g) and 2,6-bis(trifluoromethyl)-4-[3-(trifluoromethyl)pyrrolidin-3-yl]pyridine (0.195 g) in toluene was added sodium tert-butoxide (0.096 g), tris(dibenzylideneacetone)dipalladium chloroform complex (0.010 g) and xantphos (0.017 g) and the vessel was applied by Ar gas. The vessel was sealed and applied to microwave reactor at 120° C. for 10 min. The mixture was cooled to room temperature and then poured into water, which was then extracted twice with ethyl acetate. The organic layer was combined, which was then washed with water and dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the solvent was distilled away under the reduced pressure, and the residue was then purified by silica gel chromatography to yield N-[(1S)-1-(4-{3-[2,6-bis(trifluoromethyl)pyridin-4-yl]-3-(trifluoromethyl)pyrrolidin-1-yl}phenyl)ethyl]cyclopropanecarboxamide (0.272 g).

출처