24686-78-0, 1-Benzoylpiperidin-4-one is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
A 500 mL single-necked, round-bottomed flask was equipped with a heating/cooling bath, magnetic stirrer and stir bar, Dean-Stark trap, condenser, and nitrogen inlet. A solution containing N-benzoyl-4-piperidone (40.1 g, 197 mmol), pyrrolidine (37.9 g, 533 mmol), and toluene (200 mL) was refluxed for 4.5 hours under nitrogen. About 6 mL of water had collected in the trap. The volatiles were removed under reduced pressure, chasing sequentially with ethanol (45 mL) and toluene (45 mL), giving a reddish-brown residue. This residue was transferred into a 1 L single-necked, round-bottomed flask with dichloromethane (180 mL), the flask was fitted with a thermocouple and rubber septum, and a solution of phenyl isocyanate (23.97 g, 201 mmol) in dichloromethane (35 mL) was added drop-wise via syringe, keeping the temperature below 32° C. Once the addition was complete, the batch was stirred at ambient temperature for 16 hours. Volatiles were again removed under vacuum to provide a residue (89 g). This material was taken-up in methanol (165 mL) and 12 N hydrochloric acid (50 mL). The resulting mixture was stirred for 4.5 hours, diluted with water (750 mL), and extracted into chloroform (1×200 mL; 2×150 mL). The combined organic layers were dried over anhydrous sodium sulfate (50 g), filtered, and concentrated to an orange semisolid (73 g). Concentrated sulfuric acid (95 mL) was carefully added to the residue over 25 minutes, affording a brown syrup, which was heated to 100° C. for 30 minutes. The hot batch was transferred to a 2 L thick-walled conical flask, using 1,4-dioxane (65 mL) to complete the transfer. A large magnetic stir bar was introduced, followed by water (1000 mL), which was added drop-wise over 2 hours with vigorous stirring. The flask wall was scraped as needed to facilitate mixing. In this fashion, an amber solid was obtained. The solid was collected on a filter, rinsed with water (3×80 mL), and re-slurried in water (210 mL) and 37percent ammonium hydroxide (6 mL) for 40 minutes. The solid was collected on a filter (slow) and dried in a vacuum oven at 50° C. to constant weight. The title compound was obtained as an amber solid (45.1 g, 75.2percent yield) of 94.4percent purity by HPLC analysis, 24686-78-0
The synthetic route of 24686-78-0 has been constantly updated, and we look forward to future research findings.
Reference：
Patent; Allergan, Inc.; Hull, III, Clarence Eugene; Malone, Thomas C.; (30 pag.)US9255096; (2016); B1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem