Method for preparing 2-nitro-4-methylsulfonylbenzoic acid through indirect electro-oxidation
A technology of thiamphenicol benzoic acid and thiamphenicol toluene, which is applied in the field of indirect electrooxidation to prepare o-nitro-p-thiamphenicol benzoic acid, can solve the problems of easy decomposition, weak hydrogen peroxide oxidation ability, and large amount of hydrogen peroxide, and avoid Environmental pollution problems, oxidant cost savings, and high raw material utilization
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[0018] Example 1:
[0019] Indirect electrooxidation preparation of o-nitro-p-methylsulfonyl benzoic acid
[0020] Add 43g sulfuric acid with a concentration of 6mol / L and 4g chromium trioxide into a 250ml reactor. The reactor is connected with a stirring device, a thermometer, and a condenser. Turn on stirring and heating. When the temperature rises to 90°C, add 4.3g o-nitro-p-methylsulfonyltoluene and react at this temperature for 6 hours. Cool the reaction solution to below 30°C, filter and wash and dry to obtain a solid 3.81 g, the yield of o-nitro-p-methylsulfonyl benzoic acid is 38.68%. The filtrate after suction filtration contains Cr 3+ The mother liquor. Titration of Cr in mother liquor with ferrous ammonium sulfate titration 6+ After the content, the mother liquor is sent to the electrolytic cell for electrolysis. The electrolyzer is a self-made plate and frame electrolyzer, the ratio of length to height of the anode and cathode chamber is 6:1:9, the membrane used is c...
Example Embodiment
[0021] Example 2:
[0022] Indirect electrooxidation preparation of o-nitro-p-methylsulfonyl benzoic acid
[0023] Add 43g of sulfuric acid with a concentration of 7mol / L and 8g of chromium trioxide into a 250ml reactor. The reactor is connected with a stirring device, a thermometer, and a condenser. Turn on stirring and heating. When the temperature rises to 90°C, add 4.3g of o-nitro-p-methylsulfonyltoluene and react at this temperature for 6 hours. Cool the reaction solution to below 30°C, filter and wash and dry to obtain a solid 3.65 g, the yield of o-nitro-p-methylsulfonyl benzoic acid is 42.65%. The filtrate after suction filtration contains Cr 3+ The mother liquor. Titration of Cr in mother liquor with ferrous ammonium sulfate titration 6+ After the content, the mother liquor is sent to the electrolytic cell for electrolysis. The electrolyzer is a self-made plate and frame electrolyzer, the ratio of length to height of the anode and cathode chamber is 6:1:9, the membrane ...
Example Embodiment
[0024] Example 3:
[0025] Indirect electrooxidation preparation of o-nitro-p-methylsulfonyl benzoic acid
[0026] Add 103.2g of sulfuric acid with a concentration of 7mol / L and 16g of chromium trioxide into a 250ml reactor. The reactor is connected with a stirring device, a thermometer and a condenser. Turn on stirring and heating. When the temperature rises to 90°C, add 17.2g of o-nitro-p-methylsulfonyltoluene and react at this temperature for 6 hours at a constant temperature. Cool the reaction solution to below 30°C, filter and wash and dry to obtain a solid 15.68 g, the yield of o-nitro-p-methylsulfonyl benzoic acid is 43.28%. The filtrate after suction filtration contains Cr 3+ The mother liquor. Titration of Cr in mother liquor with ferrous ammonium sulfate titration 6+ After the content, the mother liquor is sent to the electrolytic cell for electrolysis. The electrolyzer is a self-made plate and frame electrolyzer, the ratio of length to height of the anode and cathode ...
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