FIELD: chemistry.
SUBSTANCE: invention relates to fine organic synthesis and pertains to a method for producing a composition of 5-nitro-4,6-dichlorobenzofuroxane and 4,6-dinitro-5,7-dichlorobenzofuroxane, consisting in first executing stage 1, wherefor a mixture of concentrated nitric and sulphuric acids is taken in the nitric acid : sulphuric acid ratio from 28:4 to 28:16 g/mol, 1 g/mol of 1,3-dinitro-2,6-dichloro-4-azidobenzene is added, then an aluminium oxide catalyst is added in an amount of 0.22 g/mol, stirred for 3 hours at a temperature of 25 to 40°C, then the reaction mass is diluted with ice water, thoroughly washed with water until a neutral reaction, dried; then executing stage 2, wherefor a mixture of 1,3-dinitro-2,6-dichloro-4-azidobenzene and 1,3,5-trinitro-2,6-dichloro-4-azidobenzene obtained at stage 1 is taken, a mixture of acetic and trichloroacetic acids is added in a volume ratio of 3:1, heated while stirring for 1 hour at a temperature of 125 to 130°C, then the reaction mixture is cooled to a temperature of 10 to 15°C, diluted with water, the deposition is filtered after 30 minutes, dissolved in chloroform, washed with water, the chloroform layer is filtered through a layer of calcined magnesium sulphate in order to remove water, chloroform is distilled in a vacuum, the deposition is dried in air, resulting in a composition in a weight ratio of 5-nitro-4,6-dichlorobenzofuroxane : 4,6-dinitro-5,7-dichlorobenzofuroxane from 80:20 to 20:80 depending on the ratio of nitric acid : sulphuric acid, respectively. The above composition of biologically active compounds can be used in various industries, in particular, in veterinary medicine, medicine, and in agriculture.
EFFECT: development of a method for producing a composition of 5-nitro-4,6-dichlorobenzofuroxane and 4,6-dinitro-5,7-dichlorobenzofuroxane with a quantitative yield and high purity.
1 cl, 9 dwg, 4 ex
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Authors
Dates
2022-04-25—Published
2021-03-31—Filed