831-50-5Relevant articles and documents
Preparation method of 2-chloride-5-nitrobenzoic acid
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Paragraph 0012; 0014; 0015, (2017/08/27)
The invention provides a preparation method of 2-chloride-5-nitrobenzoic acid. The preparation method comprises the following steps: mixing concentrated nitric acid and fuming sulphuric acid with the SO3 concentration of 20 percent according to the mass ratio of 1:(2-3), and controlling the temperature of the solution to be less than 10 DEG C in a mixing process; dripping 2-chloride trichlorotoluene, controlling the temperature of reaction liquid to be 0 to 10 DEG C, and continuously stirring at the end of dripping till the reaction is completed; pouring the reaction liquid into ice water, extracting with dichloromethane, washing an organic phase with a saturated sodium bicarbonate solution, and concentrating and drying to obtain 2-chloride-5-nitro trichlorotoluene; preparing concentrated sulfuric acid with the concentration of 85 weight percent, heating to 60 to 65 DEG C, adding the 2-chloride-5-nitro trichlorotoluene in batches, and preserving the heat till the reaction is completed; cooling the reaction liquid, adding water into the reaction liquid for dilution, extracting with ethyl acetate, taking an organic phase, and performing washing and concentration to obtain 2-chloride-5-nitrobenzoic acid. The technological steps are more reasonable in design and high in operability; the number of byproducts is small; the prepared product is relatively high in purity and can meet the requirement on industrial application.