METHOD FOR PRODUCING 4-N,N-DIMETHYLAMINOPYRIDINE Russian patent published in 2020 - IPC C07D213/74 

FIELD: chemistry.

SUBSTANCE: invention relates to organic chemistry and specifically to a method of producing 4-N,N-dimethylaminopyridine used as a catalyst in organic synthesis. Method involves heating 4-pyridyl trifluoromethane sulphonate in the presence of dimethylformamide by microwave irradiation for 50 minutes. 4-pyridyl trifluoromethane sulphonate and dimethylaminoformamide are used in weight ratio of 1:2. Microwave irradiation is carried out with constant stirring with radiation frequency of 2,455 MHz at 145–160 °C. Reaction mixture was poured into a thirty-fold excess of water, the resulting solution was adjusted to pH=7–10 with 25 % aqueous Na₂CO₃ and extracted three times with ethyl acetate, which amount is equivalent to amount of added water, organic layer of ethyl acetate is separated and washed with cold water in amount of 1/3 of volume of ethyl acetate, obtained ethyl acetate is dried by adding anhydrous Na₂SO₄, from which it is separated by filtration and distilled. Obtained product is purified by column chromatography using methylene chloride as the eluent.

EFFECT: disclosed method increases output of the end product.

1 cl, 1 tbl