反应详情

Methyl 2-(3,4-difluorobenzyl)piperidine-4-carboxylate (8.115 g, 30.14 mmol) was dissolved in DCM (200 mL) and DIPEA (6.30 mL, 36.16 mmol), then methyl carbonochloridate (3.3 mL, 41.91 mmol) was added. The solution was stirred at room temperature for 2 h. The reaction mixture was washed with 0.1 M HCl satd NaHCO3. The organic phase was passed through a phase separator and evaporated. The residue was redissolved in ether/pentane, 80/20, the solution washed with 1 M HCl 5 times, then with satd NaHCO3 and brine, dried over MgSO4, filtered and evaporated to yield dimethyl 2-(3,4-difluorobenzyl)piperidine-1,4-dicarboxylate (7.05 g, 71%). MS m/z 328 (M+H)+

1. washThe reaction mixture was washed with 0.1 M HCl
2. customevaporated
3. dissolutionThe residue was redissolved in ether/pentane
4. wash80/20, the solution washed with 1 M HCl 5 times
5. dry with materialwith satd NaHCO3 and brine, dried over MgSO4
6. filtrationfiltered
7. customevaporated