تفاعل #70911

معادلة التفاعل

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

المردود 100.9%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىThe vessel was sealed
2. 2
   أخرىat 120° C.
3. 3
   أخرىfor 10 min
4. 4
   استخلاصwas then extracted twice with ethyl acetate
5. 5
   غسيلwhich was then washed with water
6. 6
   تجفيفdried over anhydrous magnesium sulfate
7. 7
   ترشيحAfter the drying agent was filtered off
8. 8
   workup.DISTILLATIONthe solvent was distilled away under the reduced pressure
9. 9
   أخرىthe residue was then purified by silica gel chromatography

الإجراء التجريبي

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).

المصدر