反应 #70911

反应方程式

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

收率 100.9%

溶剂

toluene

反应条件

后处理

1. 1
   其他The vessel was sealed
2. 2
   其他at 120° C.
3. 3
   其他for 10 min
4. 4
   萃取was then extracted twice with ethyl acetate
5. 5
   洗涤which was then washed with water
6. 6
   干燥dried over anhydrous magnesium sulfate
7. 7
   过滤After the drying agent was filtered off
8. 8
   workup.DISTILLATIONthe solvent was distilled away under the reduced pressure
9. 9
   其他the residue was then purified by silica gel chromatography

实验过程

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).

来源