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ChemicalBook CAS DataBase List Valdecoxib 3'-Sulfonyl Chloride IMpurity
1373038-57-3

Valdecoxib 3'-Sulfonyl Chloride IMpurity synthesis

8synthesis methods
37928-17-9 Synthesis
5-Methyl-3,4-diphenylisoxazole

37928-17-9
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Valdecoxib 3'-Sulfonyl Chloride IMpurity

1373038-57-3
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Yield:1373038-57-3 80 g

Reaction Conditions:

with chlorosulfonic acid;iron(III) chloride;sulfuric acid at -10 - 80; for 10.5 h;Reagent/catalyst;Temperature;

Steps:

1 Example 1 Preparation of Compound of Formula 3

100 g of the compound of formula 2,300mL of concentrated sulfuric acid and 70g of anhydrous ferric chloride,well mixed,At a temperature of -10°C,Slowly add 500mL of chlorosulfonic acid,After the addition is completed,Stir for 0.5h; heat up to 80 ° C for 10h; then cool down to below 30 ° C,The reaction solution was slowly poured into 1000 mL of an ice water mixture.Dichloromethane extraction (500mL*2),The organic phase was dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated to dryness.The product containing the compound of formula 3 is obtained, about 80 g.

References:

CN108047155,2018,A Location in patent:Paragraph 0025; 0028

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