反应详情

To a N2 purged round bottomed flask containing tert-butyl 5-(2-fluoropyridin-3-yl)-3,4-dihydropyridine-1(2H)-carboxylate (673 mg, 2.418 mmol) was added 10% Pd/C (50 mg, 0.470 mmol) and EtOH (15 mL). After stirring for 5 minutes, 5N HCl in iPrOH (4.0 mL, 20.00 mmol) was added and the flask capped with a balloon of H2. After 16 hours, LC-MS shows ˜30% conversion. The balloon was refilled. After a further 5 days, LC-MS shows complete consumption of starting material. The reaction was filtered through a celite cartridge and the cartridge rinsed with DCM:10% EtOH (50 mL). The filtrate was concentrated in vacuo to give 2-fluoro-3-(piperidin-3-yl)pyridine dihydrochloride as a yellow foam. The material was carried forward without further purification.

1. customthe flask capped with a balloon of H2
2. waitAfter 16 hours
3. additionThe balloon was refilled
4. waitAfter a further 5 days
5. customconsumption of starting material
6. filtrationThe reaction was filtered through a celite cartridge
7. washthe cartridge rinsed with DCM
8. concentrationThe filtrate was concentrated in vacuo