110964-79-9Relevant articles and documents
Synthesis of 2-Nitro-4-methylsulfonylbenzoic Acid
Cheng, Chunsheng,Wei, Zhenyun,Ma, Xiaohua
, p. 3559 - 3563 (2015)
2-Nitro-4-methylsulfonylbenzoic acid was synthesized by the oxidation of 2-nitro-4-methylsulfonyl toluene with hydrogen peroxide in the presence of CuO/Al2O3, which was first used in strong acid system. Furthermore, the process of the reaction was thoroughly investigated by varying reactant molar ratio, reaction temperature and the amount of catalyst to obtain the optimum process. Meanwhile, unreacted 2-nitro-4-methylsulfonyl toluene can be recycled after simple treatment. The yield can reach 78.3 %. The method demonstrated the following advantages. Firstly, the oxidant dosage of sulfuric acid and hydrogen peroxide will be reduced greatly. Secondly, unreacted 2-nitro-4-methylsulfonyl toluene can be recycled. Thirdly, this process had good performance on safety. It will be a high-efficiency, energy-saving and environment-friendly technology to produce 2-nitro-4-methylsulfonylbenzoic acid.
Synthetic method for oxidizing 2 - nitro -4 - methylsulfonyl toluene with oxygen to generate 2 - nitro -4 - methylsulfonylbenzoic acid
-
Paragraph 0044-0047, (2021/09/21)
The invention relates to the field of fine chemical synthesis, in particular to a method for synthesizing 2 - nitro -4 - methylsulfonyl benzoic acid by oxidizing 2 - nitro -4 - methylsulfonyl toluene with oxygen. In the microchannel reactor, the catalyst is filled, oxygen is introduced, and 2 - nitro -4 - methylsulfonyltoluene is slowly introduced into the alkaline solution, wherein the oxygen is charged into the pressure maintaining 0.2 - 10 mpa, the reaction temperature is controlled to 130 - 200 °C. according to the obtained product content, and high conversion rate can be obtained. High selectivity, high content of continuous products.
Preparation method of 2-nitro-4-methylsulfonylbenzoic acid
-
Paragraph 0042-0043; 0050-0056; 0063-0068; 0075-0080, (2020/11/01)
The invention relates to a preparation method of 2-nitro-4-methylsulfonylbenzoic acid. Based on a nitric acid oxidation scheme, p-methylsulfonyltoluene is dissolved into a chloroalkane solvent, nitricacid is dropwise added into sulfuric acid with the mass fraction of 80-90wt%, a chloroalkane solution of p-methylsulfonyltoluene and a mixed acid solution are simultaneously and continuously added into a reaction system for a nitration reaction, the sulfuric acid is repeatedly used after the nitration reaction material liquid is treated, the sulfuric acid can be used both in the nitration reaction and the oxidation reaction, the sulfuric acid in the oxidation reaction can be repeatedly used, the total molar yield of the 2-nitro-4-methylsulfonylbenzoic acid can achieve more than 90%, and the content is more than 99%. By means of the method, the amount of waste acid in production of 2-nitro-4-methylsulfonylbenzoic acid can be reduced by 90% or above, the use amount of vanadium pentoxide isreduced by 90% or above, three wastes are greatly reduced, the process is safe and environmentally friendly, the amount of the three wastes is small, and the method is suitable for industrial large-scale production.
Synthesis process of mesotrione
-
Paragraph 0038-0052; 0057-0065, (2019/10/04)
Belonging to the field of herbicide original drug preparation, the invention discloses a synthesis process of mesotrione. The process includes the steps of: (1) catalytic oxidation: taking 2-nitro-4-methylsulfonyl toluene as the raw material, and adopting oxygen as the oxidant to generate 2-nitro-4-methylsulphonylbenzoic acid under the catalysis of a manganese oxide octahedral molecular sieve loaded heteropolyacid-transition metal salt; (2) acyl chlorination: subjecting 2-nitro-4-methylsulphonylbenzoic acid to acyl chlorination to generate 2-nitro-4-methylsulfonylbenzoyl chloride; (3) condensation: carrying out condensation reaction on 2-nitro-4-methylsulfonylbenzoyl chloride and 1, 3-cyclohexanedione to obtain an enol ester intermediate reaction solution; (4) rearrangement: subjecting the enol ester intermediate to enol ester rearrangement under the catalysis of a rearrangement catalyst to obtain a crude product reaction solution; and (5) refining: refining the crude product reaction solution to obtain a mesotrione finished product. The process provided by the invention optimizes the reaction conditions, the conversion rate of each step is high, the yield and purity of the product are high, the whole production process does not involve hypertoxic materials, and the safety is high.