FIELD: organic synthesis.
SUBSTANCE: invention relates to organic synthesis and concerns, in particular, an improved industrial method for producing prochlorase. This compound is used in agriculture as a fungicide against a wide range of diseases that damage crops, fruits and vegetables. The proposed method includes succeeding stages (a)-(d). At stage (a), intensive mixing of 2,4,6-trichlorophenol, water and excess dibromoethane is carried out, bringing the reaction mass to 100 ° C, evenly adding a solution of sodium hydroxide drop by drop for 6 hours, boiling the resulting mixture for 2 hours, cooling it to a temperature of 20°C and separating the preproduct 2- (2-brometoxy)-1,3,5-trichlorobenzene. At stage (b), there is intensive mixing of excess n-propylamine and the preproduct solution obtained at stage (a) at a temperature of 20°C, boiling of the reaction mixture for 6 hours at a temperature of 48 ° C, evaporation of excess n-propylamine, dissolution of the residue in ortho-xylene, purification of the reaction mass with hydrogen chloride gas, filtration of obtained suspension and isolation of an o-xylene solution of the preproduct N-(2-(2,4,6-trichlorophenoxy)ethyl)propane-1-amine. At stage (c), the triphosgene is heated in ortho-xylene to 100°C, the preproduct obtained at stage (b) is dripped with intensive stirring, at the end of the dripping, the reaction mixture is stirred when heated for 8 hours and the reaction mixture is cooled to 80°C. At stage (d), an o-xylene solution of imidazole and triethylamine is uniformly added at 80°C to the preproduct formed at stage (c), heated at least 60°C, mixing at 80°C for 3 hours, cooling the reaction mixture to room temperature and separating the prochlorase product.
EFFECT: invention makes it possible to increase the total yield of prochlorase to 62% and its purity to 99% while optimizing the process and increasing its safety.
1 cl, 3 ex
Title | Year | Author | Number |
---|---|---|---|
0 |
|
SU447398A1 | |
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|
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Authors
Dates
2023-01-30—Published
2022-02-25—Filed