METHOD OF PRODUCING TETRAMETHYL DERIVATIVES OF DIPHENYL ETHER Russian patent published in 2018 - IPC C07C41/01 C07C43/275 

FIELD: chemistry.

SUBSTANCE: method is carried out by the Ulman reaction using phenols and halobenzenes as starting materials in the presence of catalysts, followed by isolation of the final products. The reaction is carried out by boiling the reaction mixture and continuously mixing the reactants in an aprotic organic solvent medium at a molar ratio of the starting phenols to halobenzenes of 1:1 or 1:2 or 2:1 and in the presence of calcined potassium carbonate, copper iodide and crown ethers (1:4:1) for potassium carbonate, (0.05-0.1:1) for copper (I) iodide and (0.001-0.01:1) for crown ethers. The reaction of substituted phenols and substituted halobenzenes is carried out with a three-fold dose of 1/3 of the calculated total weight of each reagent: potassium carbonate, copper (I) iodide and crown ether in each step in the next time mode of application of these components: the first 1/3 part of these three reagents is introduced at the initial stage, after 4-8 hours of reaction, the second 1/3 part is introduced into the boiling medium in an aprotic solvent medium, after another 4-8 hours of reaction, the last 1/3 part of all three reagents is introduced and the reaction mass is boiled with stirring for an additional 4-8 hours, after which the desired product is isolated, including cooling the reaction mass, diluting it with water and treating with 50% sulfuric acid, extraction with toluene, treatment of toluene fractions with saturated sodium chloride, drying over calcium chloride and vacuum distillation are also performed.

EFFECT: target products with higher yields and more pure.

5 cl, 8 ex