Synthesis method for raw material drugs of dicamba
A synthesis method and technology of dicamba, which is applied in the field of synthesis of dicamba technical, can solve the problems of cumbersome post-processing operations, serious environmental pollution, and high catalyst cost, and achieve easy availability of raw materials and catalysts, high reaction yield, and post-processing Simple operation effect
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[0021] A method for synthesizing the original drug of dicamba,
[0022] Specific steps are as follows:
[0023] Add 81.5g (0.5mol) of 2,5-dichlorophenol and 200mL of tetrahydrofuran to a four-necked flask equipped with stirring, thermometer, dropping funnel, and reflux condenser (with calcium oxide drying tube), stir well, and add 61.25 g (0.6mol) acetic anhydride, slowly heated to 60-80°C, and reacted for 1.5h. After the reaction is complete, add ice water to cool down, filter, and wash with ice water to obtain a white solid that is 2,5-dichlorophenol acetate. The content is 94.4%, and the yield is 92.8%.
[0024] Add the product from the previous step (2,5-dichlorophenol acetate), 150 mL of nitrobenzene, and anhydrous ferric chloride into the three-necked flask, start stirring, slowly raise the temperature to 120°C, and react for 5 hours. After the reaction, the reaction solution was poured into a beaker filled with ice water and concentrated hydrochloric acid, and stirre...
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