Method for preparing 3,5,6-trichloro pyridine-2-sodium alcoholate without solvent
A technology of triclopyridine and sodium alkoxide, applied in 3 fields, can solve problems affecting product quality, endangering the operator's environment, etc., and achieve the effect of avoiding the use of highly toxic solvents and reducing production costs
Inactive Publication Date: 2007-05-30
EAST CHINA UNIV OF SCI & TECH +1
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Problems solved by technology
Since the reaction between trichloroacetyl chloride and acrylonitrile must be carried out in a highly toxic solvent (such as xylene, dichlorobenzene or nitrobenzene), the use of these highly toxic solvents not only endangers the operator and the environment, but also affects the quality of the product (The solvent used is difficult to remove in the reaction system)
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Embodiment Construction
[0009] The present invention will be further described below by embodiment, and its purpose is only to better understand content of the present invention. Therefore, the examples given do not limit the protection scope of the present invention.
[0010] Implementation example 1
[0011] Synthesis of 3,5,6-trichloropyridin-2-alcohol sodium:
[0012] In a three-neck flask, add 200 g of trichloroacetyl chloride, 80 g of acrylonitrile and 8 g of copper chloride, raise the temperature to 95° C., and react for 16 hours. The reactants were evaporated while hot to remove low boiling point substances, cooled, and added with aqueous sodium hydroxide solution to alkalize.
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The invention discloses a making method of 3, 5, 6-trichloropyridine-2-sodium alcoholate, which comprises the following steps: reacting trichloroacetyl chloride and acrylonitrile under copper halide at 80-100 deg.c; aromatizing in the alkali solution to obtain the product. The invention avoids operator from danger, which recycles high-toxic solvent and catalyst.
Description
technical field [0001] The invention relates to a preparation method of 3,5,6-trichloropyridin-2-alcohol sodium. Background technique [0002] 3,5,6-Trichloropyridin-2-alcohol sodium is an important chemical raw material and an important intermediate for the synthesis of various pesticides. [0003] At present, the methods for preparing 3,5,6-trichloropyridin-2-alcohol sodium can be classified into two categories: one is the "direct method", that is, using pyridine as a raw material, in the presence of a catalyst, at 350 ° C to 420 ° C Chlorination with chlorine gas directly at ℃ to obtain pentachloropyridine, then add zinc powder to acetonitrile to reduce and remove 4-position chlorine, and then hydrolyze in concentrated alkaline water to obtain the target product. This method has defects such as high requirements on equipment materials and harsh operating conditions (need water-free conditions). The other is the "cycling method", which is divided into acryloyl chloride m...
Claims
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Inventor 陶晓春张宏根李盛林蔡良珍刘建华
Owner EAST CHINA UNIV OF SCI & TECH