N-(2,6-dimethylphenyl)piperidine-4-carboxamide synthesis

Yield:109403-19-2 92%

Reaction Conditions:

with gadolinium(III) chloride in isopropyl alcohol;acetonitrile at 70; under 3975.4 Torr; for 2.16667 h;Temperature;Pressure;

Steps:

1

A, Add 0.23mol of pyridine-4-formyl-(2,6-dimethyl)aniline, 160ml of 35% isopropanol solution, 230ml of 45% acetonitrile solution, gadolinium chloride 0.13mol, raising the solution temperature 70 ° C, pressure 0.53MPa, the reaction 130min;B, reducing the solution temperature to 15 ° C, filtering, adding 180 mass fraction of 26% potassium bicarbonate solution and 300 mL of 37% trichlorethylene solution to the filtrate, precipitating the solid, filtering and concentrating the filtrate under reduced pressure to obtain a concentrate;C, the concentrate was added to 360ml mass fraction of 40% oxalic acid solution, the molecular sieve decolorization, the reaction 110min;D, adding a mass fraction of 48% sodium bisulfite solution 200ml, precipitated solid, filtered, the mass fraction of 55% nitromethane solution was washed, dehydration phosphorus pentoxide dehydration, mass fraction of 63% diethylamine solution Recrystallization gave 49.09 g of crystalline piperidine-4-formyl-(2,6-dimethyl)aniline in 92% yield.

References:

CN105906552,2016,A Location in patent:Paragraph 0019-0024; 0027; 0033