反应详情

To a solution of methyl 2-(3-fluoro-4-(trifluoromethyl)benzyl)isonicotinate (8.26 g, 26.37 mmol) in acetic acid (50 mL) was added platinum(IV) oxide (0.44 g, 1.94 mmol) and the resulting mixture hydrogenated at 5 bar in a Büchi hydrogenator for 8 h. The reaction mixture was filtered through a diatomeous earth filter carton and the catalyst washed with methanol. The solvents were evaporated, the residue dissolved in DCM and washed with 10% Na2CO3. After phase separation the aqueous layer was extracted with DCM. The combined organic layers were dried over MgSO4 and evaporated. Methyl 2-(3-fluoro-4-(trifluoromethyl)-benzyl)piperidine-4-carboxylate (8.4 g, 100%) was isolated as a pale yellow oil that partially solidified upon standing. MS m/z 320 (M+H)+

1. filtrationThe reaction mixture was filtered through a diatomeous earth
2. filtrationfilter carton
3. washthe catalyst washed with methanol
4. customThe solvents were evaporated
5. dissolutionthe residue dissolved in DCM
6. washwashed with 10% Na2CO3
7. customAfter phase separation the aqueous layer
8. extractionwas extracted with DCM
9. dry with materialThe combined organic layers were dried over MgSO4
10. customevaporated