Potassium Carbonate → HCID 18538581, compound

Participants

Reaction Steps

To a solution of 4-(4-fluorobenzyl)piperidine (4.25 g, 22.0 mmol) in DMF (50 mL) were added 2-chloro-N-(3,4-dichlorophenyl)acetamide (Reference Example 70-1, 4.77 g, 20.0 mmol) and potassium carbonate (3.04 g, 22.0 mmol), successively, and the mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated under reduced pressure, and to the concentrate was added ethyl acetate (70 mL). The organic layer was washed with water (20 mL, 10 mL×2), saturated sodium chloride solution (10 mL), successively, dried over magnesium sulfate and concentrated under reduced pressure. To the concentrate was added a mixed solvent of diisopropyl ether/diethyl ether (2/1)(30 mL), and the resulting precipitates were collected by filtration. The precipitates were washed with diisopropyl ether (15 mL×4), and dried under reduced pressure to give the titled compound (5.90 g) as white crystals. The filtrate was concentrated. To the concentrate was added a mixed solvent of diisopropyl ether/diethyl ether (2/1)(15 mL), and the resulting precipitates were collected by filtration. The precipitates were washed with diisopropyl ether (5 mL×4), and dried under reduced pressure to give the titled compound (1.20 g) as white crystals. Yield: 7.10 g, 90%, 7.10 g, 18.0 mmol.

Provenance & Evidence