22963-62-8Relevant academic research and scientific papers
Preparation method of 2,3,5,6-tetrachloro-4-methylsulfonyl pyridine
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Paragraph 0037; 0038-0050, (2018/12/02)
The invention discloses a preparation method of 2,3,5,6-tetrachloro-4-methylsulfonyl pyridine. The preparation method comprises the following steps: dissolving pentachloropyridine in tetrahydrofuran,dropwise adding an aqueous solution of sodium methyl mercaptide at a normal temperature, and separating phases and carrying out atmospheric distillation after reaction to recover tetrahydrofuran to obtain an organic phase; and adding organic acid and a catalyst into the organic phase, dropwise adding hydrogen peroxide in stages, and carrying out cooling and crystallization after reaction to obtainthe target product 2,3,5,6-tetrachloro-4-methylsulfonyl pyridine. According to the preparation method provided by the invention, the problems of difficult product separation and purification, high production cost, large amount of three wastes, large foul smell of intermediates, expensive oxidant and the like in the prior art are solved; an green oxidant is adopted, so that secondary pollution tothe environment is not caused; the reaction conditions are optimized, so that the purity and the yield of the target product are effectively improved; moreover, oxidant raw materials are cheap and easy to obtain, the selectivity is good, the side reactions are few, the product yield is high, the reaction conditions are mild and easy to control, and the process operation is simple and easy to industrialize.
Production method for 2,3,5,6-tetrachloro-4-(methylsulfonyl)pyridine
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Paragraph 0017; 0018; 0021; 0024; 0027; 0030; 0033; 0034, (2017/08/02)
The invention discloses a production method for 2,3,5,6-tetrachloro-4-(methylsulfonyl)pyridine, and relates to an optimizing condition of a substitution-oxidization two-step reaction. The production method comprises the following steps: adding a catalyst into pentachloropyridine serving as a raw material; dissolving the raw material in a solvent, and performing a one-step substitution reaction with a sodium methyl mercaptide aqueous solution at the room temperature to generate 2,3,5,6-tetrachloro-4-methylthiopyridine; dissolving the 2,3,5,6-tetrachloro-4-methylthiopyridine in dichloromethane; adding an oxidant and oxidizing at the room temperature to generate a target product, namely, 2,3,5,6-tetrachloro-4-(methylsulfonyl)pyridine. The product purity can be up to 99 percent through a simple purifying step after finishing the reaction, the total yield of the two-step reaction is 90 percent or above; and high guidance is given to industrial production.
