1435-48-9Relevant articles and documents
Environment-friendly production process of 2, 4-dichloro-5-fluorobenzoyl chloride
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Paragraph 0063-0068, (2020/08/22)
The present invention relates to the field of chemistry, and particularly provides a preparation method of 2, 4-dichloro-5-fluorobenzoyl chloride. According to the invention, dimerization by-productsof the 2, 4-dichloro-5-fluorobenzoyl chloride produced by a carbon tetrachloride method are subjected to alkaline hydrolysis under the action of a catalyst, then after acidification, the processed product reacts with trichloride generated by condensation of a main reaction to be converted into 2, 4-dichloro-5-fluorobenzoyl chloride, and the yield reaches over 99.8%.
Synthesis method of 2, 4-dichlorofluorobenzene
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Paragraph 0030-0033, (2019/07/04)
The invention discloses a synthetic method of 2, 4-dichlorofluorobenzene. The method comprises the following steps: 1,2,4-trichlorobenzene is used as a raw material, a calix[6]arene and trimethylolpropane borate compound is used as a phase transfer catalyst, spray-dried potassium fluoride is used as a fluorinating agent, and the 2,4-dichlorofluorobenzene is produced through one step of reaction; herein, the molar ratio of trimethylolpropane borate to potassium fluoride is 1:10-1:20, preferably 1:15; the molar ratio of the potassium fluoride to the 1,2,4-trichlorobenzene is 1:1.1; the calix[6]arene is p-tert-butyl calix[6]arene; and the molar ratio of the p-tert-butyl calix[6]arene to the 1,2,4-trichlorobenzene is 0.001:1-0.05:1, preferably 0.02:1. By using the calixarene and trihydroxymethyl borate composite catalyst, the catalytic efficiency is greatly improved, and the product yield is as high as 92%. The boiling point of the 2,4-dichlorofluorobenzene is 168-169 DEG C, the boiling point of the raw material 1,2,4-trichlorobenzene is 214 DEG C, and the boiling point of the solvent sulfolane is 285 DEG C, so that the product is simple to separate and purify. The method has the advantages of one-step synthesis, short reaction route, avoidance of nitrification and high-temperature chlorination, safer synthesis process and suitability for industrial production.
O-dichlorobenzene with a quinolone drugs for coproduction method of key intermediate
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, (2017/01/19)
The invention relates to the field of methods for preparing medicinal intermediates, in particular to the field of methods for preparing key intermediates of quinolone medicines, and develops a method for coproducing the key intermediates of the quinolone medicines by using o-dichlorobenzene as a raw material. The method comprises the following steps of: nitrifying the o-dichlorobenzene serving as the raw material, and performing distillation, purification and stepwise crystallization to obtain 2,3-dichloronitrobenzene and 3,4-dichloronitrobenzene; performing fluoridation on the 2,3-dichloronitrobenzene to obtain 3-chloro-2-fluoronitrobenzene, performing chlorination to obtain 2,6-dichlorofluorobenzene, performing nitration to obtain 1,3-dichloro-2-fluoro-4-nitrobenzene, and finally performing fluoridation to obtain 2,3,4-trifluoronitrobenzene; and performing fluoridation on the 2,3,4-trifluoronitrobenzene to obtain 3-chloro-4-fluoronitrobenzene, performing chlorination to obtain 1,3-dichloro-4-fluorobenzene, and finally performing acylation reaction on the 1,3-dichloro-4-fluorobenzene and acetylchloride to obtain 2,4-dichloro-5-fluoroacetophenone.