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ChemicalBook CAS DataBase List 2-Nitro-4-methylsulfonylbenzoic acid

2-Nitro-4-methylsulfonylbenzoic acid synthesis

6synthesis methods
3185-99-7 Synthesis
1-Methyl-4-(methylsulfonyl)-benzene

3185-99-7
278 suppliers
$5.00/10g

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Yield:110964-79-9 98%

Reaction Conditions:

Stage #1:Methyl p-tolyl sulfone with nitric acid in dichloromethane at 10;Large scale;
Stage #2: with vanadium(V) oxide;sulfuric acid at 140;Large scale;

Steps:

1-4 Example 1
A method for preparing 2-nitro-4-methylsulfonylbenzoic acid, the preparation method comprising the following steps: In the nitrification reactor, 1.0 ton of dichloromethane was added, 0.8 ton of p-methylsulfone toluene was added, and the mixture was cooled to 10 ° C. The concentrated nitric acid was added dropwise, and the sample was analyzed by hollow sampling. After the nitration reaction was completed, it was placed in an oxidation reactor. Heating, distilling off dichloromethane, then adding 70% sulfuric acid as solvent, adding catalyst vanadium pentoxide, heating to 140 ° C, adding 60% nitric acid for oxidation reaction, after the reaction is finished, cooling to 25 ° C, centrifugation, mother liquor Applying to the oxidation reaction, the crude product is put into the reaction tank again, water is added, and the alkali solution is added to adjust the alkaline pH to 11. After filtering the impurities, the mother droplet is diluted with sulfuric acid to adjust the pH to 1.9, cooled and centrifuged, and dried to obtain a fine product

References:

Jiangsu Xin Xinlong Pharmaceutical Technology Co., Ltd.;Zhou Lidong;Zhou Jialin;Zhang Lan;Jiang Nan;Zhang Qin;Ji Zugen CN109503437, 2019, A Location in patent:Paragraph 0020-0033

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