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ChemicalBook CAS DataBase List N-PHENYLPIPERIDINE-4-CARBOXAMIDE

N-PHENYLPIPERIDINE-4-CARBOXAMIDE synthesis

7synthesis methods
-

Yield:73415-85-7 96%

Reaction Conditions:

with hydrogenchloride in 1,4-dioxane at 5 - 10;Inert atmosphere;

Steps:

3 Step 3

Step 3: To a 50 mL single neck round-bottomed flask containing (1 g, 3.286 mmol) the material from step 2) at 5-10 °C, was added 1,4-dioxane (25 mL), under nitrogen and started stirring. Hydrochloric acid in dioxane (3.0 g, 16.43 mmol) was added drop wise so that the temperature does not raise above 5-10 °C. After complete addition, the contents were stirred and allowed to attain room temperature slowly, during which time solid formation was observed. The reaction was checked for its progress by LCMS and found to be complete. The organics were distilled off and the residual material was taken in dichloromethane and stirred well, during which time some solid started to separate out. This was filtered off and the dichloromethane layer was dried and evaporated under vacuum to get 0.402 g (96%) of N-phenylpiperidine-4-carboxamide as off-white solid, which was confirmed by JH NMR.

References:

WO2016/27284,2016,A2 Location in patent:Page/Page column 67