ChemicalBook CAS DataBase List 4-Methylsulphonylphenylacetic acid

4-Methylsulphonylphenylacetic acid synthesis

7synthesis methods

Product Name:4-Methylsulphonylphenylacetic acid
CAS Number:90536-66-6
Molecular formula:C9H10O4S
Molecular Weight:214.24

4-Methylsulphonylphenylacetic acid can be used as organic synthesis intermediate and pharmaceutical intermediate, mainly used in laboratory research and development process. 2-Bromoacetophenone, dissolved in acetonitrile, was added to Et3N, followed by 4-methylsulfonylphenylacetic acid. After 1.5 h at room temperature, 1,8-diazabicyclo[5,4,0]undec-7-ene was added. The reaction mixture was stirred for 1 h, and then treated with 1 N HCl to give 4-Methylsulphonylphenylacetic acid .

109347-44-6 Synthesis

109347-44-6
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32703-82-5 Synthesis

6-tert-Butyl-2,3-naphthalenedicarbonitrile

32703-82-5
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Yield:32703-82-5 84%

Reaction Conditions:

with sodium tungstate;dihydrogen peroxide;sodium carbonate in water;Reagent/catalyst;

Steps:

5 Example 5: Preparation of 4-Methanesulfonylphenylacetic Acid

In a 500 mL dry three-necked bottle, 50.0 g of 4-methanesulfonyl phenylacetaldehyde was added, 200 mL of water was added, and sodium carbonate was added.30g, add 0.5g of sodium tungstate under stirring,70 mL of 30% hydrogen peroxide solution was slowly added dropwise, and the reaction solution gradually became clear as the reaction proceeded.TLC test, after the end of the reaction, filtration, the filtrate was slowly added 10% hydrochloric acid, adjust the pH to 2-3, filtered,This gave crude 4-methanesulfonylphenylacetic acid.The above 4-methylsulfonylphenyl acetic acid was dissolved in 1% sodium hydroxide, and saturated sodium thiosulfate solution was added in 10 mL.After extracting 50 mL of ethyl acetate twice, 200 mL of ethyl acetate was added to the aqueous layer, and 10% hydrochloric acid was added to adjust the pH to 2-3.The ethyl acetate layer was separated. The aqueous layer was extracted once with 200 mL of ethyl acetate.Combine the ethyl acetate layers, heat to reflux, add 200 mL of n-heptane, slowly cool to 0-5 °C,The mixture was stirred at this temperature for 1 hour, filtered and vacuum dried to give 54.2 g of 4-methanesulfonylphenylacetic acid. Yield: 84.0%.

References:

CN107556223,2018,A Location in patent:Paragraph 0038-0045