15854-73-6Relevant articles and documents
Mild and Robust Stille Reactions in Water using Parts Per Million Levels of a Triphenylphosphine-Based Palladacycle
Takale, Balaram S.,Thakore, Ruchita R.,Casotti, Gianluca,Li, Xaiohan,Gallou, Fabrice,Lipshutz, Bruce H.
supporting information, p. 4158 - 4163 (2021/02/01)
An inexpensive and new triphenylphosphine-based palladacycle has been developed as a pre-catalyst, leading to highly effective Stille cross-coupling reactions in water under mild reaction conditions. Only 500–1000 ppm of Pd suffices for couplings involving a variety of aryl/heteroaryl halides with aryl/hetaryl stannanes. Several drug intermediates can be prepared using this catalyst in aqueous nanoreactors formed by 2 wt % Brij-30 in water.
Synthetic method for bifenazate
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Paragraph 0027-0032, (2019/08/12)
The invention relates to a synthetic method for bifenazate. The method comprises the following specific synthetic sections: step 1, performing nitration: mixing a 4-hydroxybiphenyl solution and a toluene solution under stirring for a reaction, and adding a HNO3 solution dropwise for a reaction to obtain a nitration reaction solution; step 2, performing methylation: mixing the nitration reaction solution and anhydrous sodium carbonate powder for a reaction, and adding a dimethyl carbonate solution dropwise for a reaction to obtain a methylation reaction solution; step 3, performing hydrogenation: throwing the methylation reaction solution, hydrogen gas, and Raney nickel into a reaction kettle for a reaction to obtain a hydrogenation reaction liquid; step 4, performing hydrazination: performing a primary hydrazination reaction, performing a secondary hydrazination reaction, performing filter pressing, performing a tertiary hydrazination reaction, and performing secondary filter pressingto obtain a condensation reaction liquid; step 5, performing condensation: mixing a third hydrazine compound, an ethyl acetate solution and an isopropyl chloroformate solution for a reaction to obtaina bifenazate mixed liquid; and step 6, performing purification: performing desolvation, performing crystallization, performing centrifugation, performing washing, performing secondary centrifugation,and performing drying to obtain the finished bifenazate. The method provided by the invention has the effect of improving purity of the bifenazate product.
Compounding method for acaricide bifenazate intermediate 3-nitro-4-methoxyphenyl
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Paragraph 0028-0049, (2019/02/10)
The invention relates to a compounding method for an acaricide bifenazate intermediate 3-nitro-4-methoxyphenyl and belongs to the field of pesticide preparation. The compounding method is characterized by acquiring 3-nitro-4-methoxyphenyl from the reaction of 4-halogenated-2-nitroanisole and benzene halide under the action of catalyst. The reaction process is as follows: 1) uniformly mixing 4-halogenated-2-nitroanisole, benzene halide, catalyst and solvent A under a shielding gas condition, rising temperature to 130-150 DEG C, controlling pressure to 7-12 barometric pressures, reacting for 20-35h and ending; 2) performing vacuum filtration on the system and removing solid insoluble substances, thereby acquiring a filtrate a; pouring the filtrate a into 3-5 times of water, adding a solventB for extracting, layering and then using a drying agent for drying an organic phase, and concentrating, thereby acquiring a solid; re-crystallizing the solid with a solvent C, thereby acquiring 3-nitro-4-methoxyphenyl. The compounding method has the advantages of few steps, higher yield and more convenient operation.