反应详情

Dimethyl 2-(4-(trifluoromethyl)benzyl)piperidine-1,4-dicarboxylate (10.9 g, 30.33 mmol) was dissolved in acetonitrile (80 mL) and water (1.6 mL), then lithium bromide (21.07 g, 242.67 mmol) and triethylamine (16.82 mL, 121.33 mmol) were added and the resulting yellow suspension was heated at reflux. Water (60 mL) and MTBE were added. The organic phase was extracted with water (×2). To the pooled aqueous layer was added MTBE and the solution was acidified to pH 1 with HCl and then extracted with MTBE (×2). The organic layer was dried Na2SO4, filtered through celite and the solvent evaporated to yield 1-(methoxycarbonyl)-2-(4-(trifluoromethyl)benzyl)piperidine-4-carboxylic acid (9.14 g, 87%).

1. temperaturethe resulting yellow suspension was heated
2. temperatureat reflux
3. extractionThe organic phase was extracted with water (×2)
4. additionTo the pooled aqueous layer was added MTBE
5. extractionextracted with MTBE (×2)
6. filtrationfiltered through celite
7. customthe solvent evaporated