反应详情

To a solution of 3-(phenyl(4-(trifluoromethyl)phenyl)methyl)piperidine (1.0 g, 3.13 mmol) in MeCN (10 mL) was added triethyl amine (1.3 mL, 9.4 mmol) at rt. After stirring at rt for 15 min, it was cooled to 0° C. and ethyl bromoacetate (0.62 g, 3.71 mmol) was added dropwise. After stirring at rt for 6 h, the solvent was removed under vacuum and the residue was diluted with water, extracted with ethyl acetate, the combined organic layer was dried over anhydrous sodium sulfate and concentrated under vacuum to afforded the crude product. Column chromatography (SiO2, 10-15% ethyl acetate in hexane) afforded ethyl 2-(3-(phenyl(4-(trifluoromethyl)phenyl)methyl)piperidin-1-yl)acetate (0.6 g, 48% yield) as a pale yellow solid. MS (ESI, pos. ion) m/z: 406 (M+1).

1. temperatureit was cooled to 0° C.
2. stirringAfter stirring at rt for 6 h
3. customthe solvent was removed under vacuum
4. additionthe residue was diluted with water
5. extractionextracted with ethyl acetate
6. dry with materialthe combined organic layer was dried over anhydrous sodium sulfate
7. concentrationconcentrated under vacuum
8. customto afforded the crude product