- Synthesis method of high-purity bacteriostatic agent and derivatives thereof
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The invention discloses a synthesis method of a high-purity bacteriostatic agent and derivatives thereof. The synthesis method comprises the following specific steps: adding primary amine or secondaryamine into a solvent, adding perchloromethyl mercaptan, reacting at room temperature for 14-18 hours, washing the reaction solution with water, separating, drying, concentrating the solvent and separating to obtain an intermediate 1; mixing the intermediate 1 with a solvent and fluoride, heating to 100-140 DEG C, reacting for 6-18 hours, filtering the reaction solution, washing with water, drying, concentrating the solvent, rectifying and separating to obtain an intermediate 2; mixing the intermediate 2 with a solvent, introducing hydrogen chloride gas at 0-10 DEG C to react for 2-16 hours, washing the reaction solution with water, separating, drying and concentrating the solvent to obtain an intermediate 3; and mixing the intermediate 4 with a solvent, adding alkali at 0-10 DEG C, reacting for 0.5-1 hour, adding the intermediate 3, reacting at room temperature for 1-2 hours, washing the reaction solution with water, separating, drying and concentrating the solvent to obtain the target compound. The method is low in cost and high in product yield and a high-purity product can be obtained.
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Paragraph 0089-0092
(2020/04/29)
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- N, N-dimethyl-N-phenyl-(N- fluorine two chlorine armor thio)-sulfonaide synthesis process
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The invention discloses a process for synthesizing N,N-dimethyl-N-phenyl-(N-fluorodichloromethylmercapto)-sulfamide. The synthesis process comprises the following steps: by taking ferric fluoride as a fluoride, recrystallizing a toluene solution of fluorodichloromethylsulfuryl chloride and N,N-dimethyl-N'-phenyl sulfamide under a certain reaction conditions so as to prepare the N,N-dimethyl-N-phenyl-(N-fluorodichloromethylmercapto)-sulfamide. According to the synthesis process, an intermediate is synthesized, the utilization rate and yield of the intermediate can be improved in the intermediate preparation process, the residual substances are conveniently recycled after the reaction, the cost is greatly saved, and the environmental pollution is reduced. The ferric fluoride is taken as the fluoride in the intermediate synthesis process, so that the yield of the N,N-dimethyl-N-phenyl-(N-fluorodichloromethylmercapto)-sulfamide is improved, the influence on the environment is slight, and the problems that the N,N-dimethyl-N-phenyl-(N-fluorodichloromethylmercapto)-sulfamide is difficultly produced industrially because the raw material cost is high, the generated three industrial wastes have great damage to the environment and the yield is low and instable in the conventional method and the like are solved.
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Paragraph 0079-0082; 0084; 0087; 0088
(2017/02/09)
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- 1-(trihalomethylsulfenyl)-4-aryl-1,2,4-triazolin-5-ones and fungicides containing these compounds
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1-(trihalomethylsulfenyl)-4-aryl-1,2,4-triazolidin-5-ones of the formula STR1 where R is substituted or unsubstituted alkyl, or is alkenyl or cycloalkyl, X is hydrogen, halogen, substituted or unsubstituted alkyl or alkoxy, alkenyl, cyano, nitro, or substituted or unsubstituted phenyl or phenoxy, n is an integer from 1 to 5, and Y is fluorine or chlorine, and fungicides containing these compounds.
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- Methyl-halogenated Allyl Methyl Sulfoxides and Sulfones and the Synthesis of Halogenated Sulfines
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Allyl methyl sulfoxides R1R2R3C-S(O)-CH2CH=CH2 1a-7a (R1, R2, R3 = H, F, Cl, CF3) as well as the corresponding sulfones 1b-7b were synthesized.The sulfoxides substituted at the methyl group are in equilibrium with the allyl sulfenates R1R2R3-S-OCH2CH=CH2 depending on temperature and kind of substitution.By pyrolysis of the sulfoxides 2a, 3a, 4a, and 7a the sulfines Cl2C=SO and (CF3)2C=SO could be prepared, and evidence for the existence of the sulfines ClFC=SO and F2C=SO could be obtained.The new pentenes 12 and 14 are described.
- Holoch, Jan,Sundermeyer, Wolfgang
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p. 269 - 278
(2007/10/02)
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- N'-Sulfenyl-N"-dihalophenylimidazolidinediones
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3-(3',5'-Dihalophenyl)-1-sulfenylimidazolidine-2,4-diones of the formula: STR1 wherein X is a chlorine atom or a bromine atom, Y1, Y2 and Y3 are each a chlorine atom or a fluorine atom and R1 and R2 are individually a hydrogen atom or a methyl group, which show high microbicidal activities against various fungi without any material toxicity to mammals and plants and can be produced by reacting the corresponding 1-unsubstituted compound with a sulfenyl halide.
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