ChemicalBook CAS DataBase List Azilsartan iMpurity A

Azilsartan iMpurity A synthesis

3synthesis methods

Product Name:Azilsartan iMpurity A
CAS Number:147404-76-0
Molecular formula:C25H23N3O4
Molecular Weight:429.47

147403-65-4 Synthesis

(Z)-Methyl 2-ethoxy-3-((2'-(N'-hydroxycarbaMiMidoyl)biphenyl-4-yl)Methyl)-3H-benzo[d] iMidazole-4-carboxylate

147403-65-4
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147404-76-0
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Yield:147404-76-0 85%

Reaction Conditions:

with 1,1'-carbonyldiimidazole in 1,4-dioxane for 5 h;Reflux;Solvent;

Steps:

1 Example 1
10.0 g (22.5 mmol) of Intermediate II was added to 100 ml of 1,4-dioxane, heated to reflux,A solution of 3.84 g (23.7 mmol, 1.05 eq) of carbonyldiimidazole in 50 ml of 1,4-dioxane was slowly added dropwise,After completion of the dropwise addition, the reaction was refluxed for 5 hours; the reaction was stopped and the solvent was distilled off under reduced pressure;The residue was dissolved in ethyl acetate and added with water. Under stirring, HCl was adjusted to pH 3, allowed to stand for delamination,The aqueous phase was removed; water was added for washing, the aqueous phase was separated off and the organic phase was washed with saturated brine,The aqueous phase was removed and the organic phase was cooled with an ice-water bath to cool and crystallize for 1 hour, filtered, washed with a small amount of ethyl acetate,Impurity A was obtained in a yield of 85%

References:

Shandong Xinhua Pharmaceutical Co., Ltd.;Wu Hui;Zheng Zhonghui;Wang Jun;Shen Hong;Xu Ling CN105924400, 2016, A Location in patent:Paragraph 0024; 0025; 0031

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139481-44-0 Synthesis