METHOD OF OBTAINING DINITROPROTECTIVE DIPHENYL AND TRIPHENYL ETHERS Russian patent published in 2018 - IPC C07C201/12 C07C205/38 

FIELD: chemistry.

SUBSTANCE: invention relates to a method for producing dinitro derivatives of diphenyl and triphenyl ethers. Method is carried out by reaction of interaction of substituted phenol with para-chloronitrobenzene in the medium of an organic solvent in inert gas atmosphere at elevated temperature in the presence of a catalyst, followed by isolation of the target product. Method is characterized in that the reaction of the interaction of para-chloronitrobenzene with a substituted phenol selected from the group of para-nitrophenol and hydroquinone is carried out in aprotic organic solvent with a molar ratio of starting phenols to para-chloronitrobenzene, equal to 1:1, or 1:2, or 2:1, in the presence of calcined potassium carbonate, copper (I) iodide and crown ethers, taken in amounts corresponding to their molar ratio to phenols, respectively (1–4:1) – for potassium carbonate, (0.05–0.1:1) – for copper (I) iodide and (0.001–0.01:1) – for crown ethers. Reaction of the interaction of substituted phenols with para-chloronitrobenzene is carried out when dosed three times into reaction mass at each stage, 1/3 of the calculated total weight of each of the listed reagents – potassium carbonate, copper (I) iodide and crown-ether – in the next timed mode of introduction of these components: the first 1/3 of these three reagents are injected at the initial stage, after 4–8 hours of carrying out the reaction while boiling in the medium of aprotic solvent, the second 1/3 part is injected, after another 4–8 hours of carrying out the reaction in the same mode, the last 1/3 part of all three reagents is injected and reaction mass is boiled with 4–8 hours Thereafter, the desired product is isolated, including cooling the reaction mass, diluting it with water and treating with 50 % sulfuric acid, extracting with toluene, treating the toluene fractions with saturated sodium chloride, drying over calcium chloride and vacuum distillation.

EFFECT: proposed method allows to obtain dinitro derivatives of diphenyl and triphenyl ethers with higher yields.

3 cl, 8 ex