111992-16-6Relevant articles and documents
Method for preparing sulfentrazone intermediate
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Paragraph 0143-0148, (2021/01/04)
The invention relates to the field of pesticides, in particular to a method for preparing a sulfentrazone intermediate. The method comprises the steps that in the presence of water and a first organicsolvent, a compound with the structure shown in the formula (II) and chlorine are subjected to a contact reaction, X and Y are independently selected from H and Cl, and X and Y are not Cl at the sametime; R is H or difluoromethyl; the contact reaction comprises an oxidation contact reaction and a chlorination contact reaction in sequence, and the conditions of the oxidation contact reaction areas follows: the temperature is 5-35 DEG C, and the time is 30-120 minutes; and the conditions of the chlorination contact reaction are as follows: the temperature is 40-90 DEG C, and the time is 3-6 hours. According to the method, the yield and the purity of the sulfentrazone intermediate with the structure shown in the formula (I) can be effectively improved, and the method is easy to operate andmore environmentally friendly.
Synthesizing method of sulfentrazone
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, (2019/02/08)
The invention discloses a synthesizing method of sulfentrazone. The synthesizing method comprises the following steps of using a compound (II) as the raw material, and performing difluoro methylation,chlorination and bromination; then, performing methylsulfonylation, so as to obtain the final product of the sulfentrazone. The synthesizing method has the advantages that the obtained intermediate after chlorination is firstly brominated, and then the obtained intermediate after bromination and the methanesulfonamide are catalyzed by a catalyst to obtain the sulfentrazone; the chemical selectivity is high, and the dangerous technologies of nitrification, hydrogenation and the like in the traditional technology route are avoided; the production of a large amount of waste acid and waste waterin the nitrification process is avoided, the green effect is better, the efficiency is higher, and the safety and reliability are higher; the whole technology is simple and convenient, and the reaction conditions are mild; by adjusting the reaction conditions, the yield rate of the obtained product is high, the quality of the product is high, and the synthesizing method is suitable for industrialized production.
Method for synthesizing 1-(2,4-dichlorophenyl)-3-methyl-4-difluoromethyl-1,2,4-triazole-5-ketone
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, (2018/03/28)
The invention discloses a method for synthesizing 1-(2,4-dichlorophenyl)-3-methyl-4-difluoromethyl-1,2,4-triazole-5-ketone. The method takes p-chloroaniline as a raw material, through diazotization, reduction, and salt forming, p-chlorophenylhydrazine hydrochloride is synthesized, p-chlorophenylhydrazine is obtained through alkali neutralization, under condition that tert-butyl alcohol is taken asa solvent, chlorophenylhydrazine, acetaldehyde, sodium cyanate and sodium hypochlorite are subjected to condensation, cyclisation and an oxidation reaction to generate 1-p-chlorophenyl-3-methyl-1H-1,2,4-triazole-5-ketone, and the 1-p-chlorophenyl-3-methyl-1H-1,2,4-triazole-5-ketone is subjected to salt forming, reaction with chlorodifluoromethane, and chlorination to obtain the 1-(2,4-dichlorophenyl)-3-methyl-4-difluoromethyl-1,2,4-triazole-5-ketone (a sulfentrazone intermediate). The synthetic method takes p-chloroanniline as the raw material, the synthetic method is realized by only one-time chlorination, steric hindrance for intermediate synthesis is small, and the impurity is low, so that the yield is increased; in addition, the raw materials required by the synthesis route are easilyacquired, the cost is low, the condition is mild, operation is simple, security is high, and the synthesis method is in favor of realizing industrial production.
