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US 2014/0194630 A1Published application
Process for synthesis of fipronil
OwnerKeki Hormusji Ghardainventor
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Abstract
A process for preparation of Fipronil (i.e. 5-amino-1-(2, 6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoro-methylsulphinyl-pyrazole) is provided, which comprises oxidizing 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-tri-fluoromethylthio-pyrazole with sulfuric acid and hydrogen peroxide as oxidizing agent in the presence of a solvent such as ethylene dichloride, chlorobenzene.
Claims5
A process for preparing fipronil, said process comprising the following steps:
- a. oxidizing, in a solvent selected from the group consisting of ethylene dichloride, methylene dichloride, carbon tetrachloride, chloroform, dibromoethane, bromobenzene, chlorobenzene and ortho-dichlorobenzene, a reactant mixture containing a compound 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoro methyl thio-pyrazole of formula II and concentrated sulfuric acid having concentration in the range of 75% to 98% w/w, with hydrogen peroxide having concentration in the range 40 to 70% w/w, at a temperature in the range of -10° C. to 40° C. to obtain an oxidized product mixture;
- b. quenching said product mixture with water at a temperature in the range of 10 to 25° C.;
- c. heating the quenched product mixture at a temperature in the range of 60 to 70° C. to obtain a biphasic system containing an aqueous phase containing sulphuric acid and an organic phase containing the oxidized product;
- d. isolating said organic phase by separating the aqueous phase;
- e. neutralizing the isolated organic phase containing the oxidized product to obtain crude fipronil;
- and
- f. crystallizing the crude fipronil to obtain crystallized fipronil.
4 more elements
Dependencies are inferred from the claim text.