反应详情

Dimethyl 2-(4-fluorophenethyl)piperidine-1,4-dicarboxylate (3.18 g, 9.83 mmol) was dissolved in acetonitrile (35 mL) and water (0.7 mL) and lithium bromide (6.83 g, 78.67 mmol) was added. Triethylamine (5.45 mL, 39.34 mmol) was added and the resulting suspension was heated under reflux for 5 h. MTBE and water were added, the phases separated and the organic layer was extracted with water. The combined aqueous layers were acidified to pH 1 with 3.8 M HCl and extracted with MTBE. The combined organic layers were washed with water, dried with Na2SO4 and evaporated. Crude 2-(4-fluorophenethyl)-1-(methoxycarbonyl)piperidine-4-carboxylic acid (4.37 g) was isolated. MS m/z 310 (M+H)+

1. temperaturethe resulting suspension was heated
2. temperatureunder reflux for 5 h
3. customthe phases separated
4. extractionthe organic layer was extracted with water
5. extractionextracted with MTBE
6. washThe combined organic layers were washed with water
7. dry with materialdried with Na2SO4
8. customevaporated