반응 #70908

반응 방정식

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

3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidine

sodium t-butoxide

toluene

→

N-[(1S)-1-(4-{3-[3,5-bis-(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}phenyl)ethyl]cyclopropanecarboxamide

수율 100.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타reacted in a microwave reactor (Initiator™, manufactured by Biotage) for 10 minutes at 120° C
2. 2
   workup.ADDITIONwas added
3. 3
   여과the precipitates were filtered
4. 4
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
5. 5
   기타the residue was purified by silica gel column chromatography

실험 절차

To a reaction vessel, N-[(1S)-1-(4-bromophenyl)ethyl]cyclopropanecarboxamide (134 mg), 3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidine (211 mg), sodium t-butoxide (96 mg), tris(dibenzylideneacetone)dipalladium(0)-chloroform adduct (10 mg), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (18 mg) and toluene (6 ml) were added, and reacted in a microwave reactor (Initiator™, manufactured by Biotage) for 10 minutes at 120° C. Upon the completion of the reaction, ethyl acetate was added and the precipitates were filtered by using silica gel. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography to obtain N-[(1S)-1-(4-{3-[3,5-bis-(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}phenyl)ethyl]cyclopropanecarboxamide (269 mg). 1H-NMR (CDCl3) as given in Table 2

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