Preparation method of 2-nitro-4-methyl sulfone benzoic acid
A technology of thiamphenicol benzoic acid and thiamphenicol toluene, which is applied in the field of one-pot synthesis of 2-nitro-4-thiamphenicol benzoic acid, which can solve incomplete reaction, large amount of three wastes, and difficult oxidation, etc. problems, to achieve the effect of improving oxidation capacity, simplifying production process and reducing acidic wastewater
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Embodiment 1
[0027] 1. Preparation of oxidizing agent
[0028] Put 136g of concentrated sulfuric acid in a three-necked flask, and slowly add 68.0g (0.6mol) of 30% hydrogen peroxide solution dropwise therein under magnetic stirring. Heat will be released during the dropwise addition, and the temperature should be controlled below 30°C. , continue to stir for 20 min after the dropwise addition, and set aside.
[0029] 2, Preparation of 2-nitro-4-thiamphenicol benzoic acid
[0030] Add 17.02g (0.1mol) of 4-thiamphenicol toluene and 88.3g (0.883mol) of concentrated sulfuric acid into the three-necked flask, place the three-necked flask in a water bath, and slowly add 10.18g (0.105mol) of concentrated nitric acid dropwise to the three-necked flask. ), stirring constantly, and controlling the reaction temperature between 0 and 15°C, the dripping was completed in about 2.5 hours, and the reaction was continued for 0.6 hours after the addition was completed. If the nitration product is not sepa...
Embodiment 2
[0032] 1. Preparation of oxidizing agent
[0033] The concentrated sulfuric acid of 237.9g is placed in the there-necked flask, and under magnetic stirring, slowly add 79.3g (0.7mol) concentration of 30% aqueous hydrogen peroxide solution therein, heat will be released during the dropping process, control the temperature at 30°C Next, continue to stir for 20 minutes after the dropwise addition is completed, and set aside.
[0034] 2, Preparation of 2-nitro-4-thiamphenicol benzoic acid
[0035] Add 17.02g (0.1mol) of 4-thiamphenicol toluene and 97.1g (0.971mol) of concentrated sulfuric acid into a three-necked flask, place the three-necked flask in a water bath, and slowly add 11.24g (0.116mol) of concentrated nitric acid dropwise to the three-necked flask ), stirring constantly, and controlling the reaction temperature between 0 and 15°C, the dripping was completed in about 2.5 hours, and the reaction was continued for 0.6 hours after the addition was completed. If the nit...
Embodiment 3
[0037] 1. Preparation of oxidizing agent
[0038] Place 68.0 g of concentrated sulfuric acid in a three-necked flask, and slowly add 68.0 g (0.6 mol) of 30% aqueous hydrogen peroxide dropwise therein under magnetic stirring. Heat will be released during the dropping process, and the temperature will be controlled at 30°C. Next, continue to stir for 20 minutes after the dropwise addition is completed, and set aside.
[0039] 2, Preparation of 2-nitro-4-thiamphenicol benzoic acid
[0040]Add 17.02g (0.1mol) of 4-thiamphenicol toluene and 79.5g (0.795mol) of concentrated sulfuric acid into the three-necked flask, place the three-necked flask in a water bath, and slowly add 9.21g (0.095mol) of concentrated nitric acid dropwise to the three-necked flask. ), stirring constantly, and controlling the reaction temperature between 0 and 15°C, the dripping was completed in about 2.5 hours, and the reaction was continued for 0.6 hours after the addition was completed. If the nitration p...
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