213132-03-7Relevant articles and documents
Synthesis method of 5-amidogen-3-cyano-1-(2,6-dichloro-4-trifluoromethyl phenyl) pyrazole
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Paragraph 0050-0053; 0073-0076; 0081-0084, (2019/10/01)
The invention discloses a synthesis method of 5-amidogen-3-cyano-1-(2,6-dichloro-4-trifluoromethyl phenyl) pyrazole. The synthesis method comprises the following steps that at 0 to 5 DEG C, an ethanol solution of 2,6-dichloro-4-trifluoromethyl aniline salt and a sodium nitrite solution with the mass concentration being 40 to 45 percent are simultaneously and dropwise added into a hydrochloric acid ethanol solution of 2,3-dicyan ethyl propionate; reaction liquid is subjected to heat insulation for 2 to 12h at 0 to 5 DEG C until the concentration of 2,6-dichloro-4-trifluoromethyl aniline in the reaction liquid is smaller than or equal to 0.5 percent; reducing reagents are dropwise added into the reaction liquid to remove excessive nitrous acid in the reaction liquid until the nitrous acid in the reaction liquid is completely removed; at 10 to 15 DEG C, ammonium hydroxide and ethanol are added into the reaction liquid, so that the pH of the reaction liquid is greater than or equal to 11; heat insulation is performed for 8 to 24h. The synthesis method has the advantages that the technology prejudice of technicians in the field is broken; the cost is reduced; the generation of three wastes is greatly reduced.
