N,N-Dimethyl-2-(4-methoxyphenyl)-acetamide synthesis

8synthesis methods

Product Name:N,N-Dimethyl-2-(4-methoxyphenyl)-acetamide
CAS Number:19625-79-7
Molecular formula:C11H15NO2
Molecular Weight:193.24

104-01-8 Synthesis

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N,N-Dimethyl-2-(4-methoxyphenyl)-acetamide

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Yield: 94%

Reaction Conditions:

Stage #1:4-Methoxyphenylacetic acid;dimethyl amine at 100;Autoclave;
Stage #2: at 95 - 245; under 18751.9 Torr; for 0.0158333 h;Product distribution / selectivity;Microwave irradiation;

Steps:

5
Example 5 Preparation of N,N-dimethyl-4-methoxyphenylacetamide; While cooling with dry ice, 2.7 kg of dimethylamine (60 mol) from a reservoir bottle were condensed into a cold trap. A 10 l Büchi stirred autoclave with gas inlet tube, mechanical stirrer, internal thermometer and pressure equalizer was initially charged with 10 kg of 4-methoxyphenylacetic acid (60 mol), which were melted at about 100° C. By slowly thawing the amine-containing cold trap, gaseous dimethylamine was introduced slowly through the gas inlet tube directly into the acid melt in the stirred autoclave. In an exothermic reaction, the 4-methoxyphenyl-acetic acid N,N-dimethylammonium salt formed. The molten ammonium salt thus obtained (95° C.) was pumped continuously through the reaction tube at 3.0 l/h at a working pressure of about 25 bar and exposed to a microwave power of 1.95 kW, 95% of which was absorbed by the reaction mixture. The residence time of the reaction mixture in the irradiation zone was approx. 57 seconds. At the end of the reaction tube, the reaction mixture had a temperature of 245° C.Based on the acid component used, a conversion of 97% of theory was attained in the crude product. The crude product contained <2 ppm of iron and had a pale yellow color. After extractive removal of unconverted reactants, a virtually colorless product with 99% purity was obtained with 94% yield.

References:

CLARIANT FINANCE (BVI) LIMITED US2011/137081, 2011, A1 Location in patent:Page/Page column 8

104-01-8 Synthesis

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506-59-2 Synthesis