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ChemicalBook CAS DataBase List 3,5-Bis[(2-fluorophenyl)Methylene]-4-piperidinone

3,5-Bis[(2-fluorophenyl)Methylene]-4-piperidinone synthesis

7synthesis methods
-

Yield:342808-40-6 75 %

Reaction Conditions:

with sodium hydroxide in methanol;water at 20;

Steps:

1.2

weigh 1mmol (0.1527g) of 4-piperidone hydrochloride hydrate, measure 2mmol (0.86mL) of 2-fluorobenzaldehyde, dissolve it in 6mL of methanol, place it on a magnetic stirrer, and put The rotor should be preferably at a speed at which all liquids can be rotated, then slowly add 1.5mL 20w/w% sodium hydroxide aqueous solution dropwise to the reaction system, stir at room temperature and continue the reaction, and follow the reaction process by silica gel thin layer chromatography (TLC). After reacting for 2 hours, quickly add 1mL of 12mol/L hydrochloric acid, adjust the pH to 6, continue to react for 20 minutes, let it stand for 30 minutes, filter, take a small amount of filter residue and dissolve it in methanol to obtain a crude product solution, pass through a 0.22μm filter membrane with high performance liquid phase Chromatographic detection.Save the filter residue and wash it with methanol for several times, and check the purity by TLC and ultra-high performance liquid phase analysis. The purified sample is dried in a 37°C oven to constant weight to obtain a dry pure product.Results: The crude product solution was a yellow-green clear solution, the pure product was a light yellow powder, and the yield was 75%.

References:

CN115232068,2022,A Location in patent:Paragraph 0063; 0067-0071