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ChemicalBook CAS DataBase List XANTHENE-9-CARBOXYLIC ACID

XANTHENE-9-CARBOXYLIC ACID synthesis

9synthesis methods
85554-24-1 Synthesis
XANTHENE-9-CARBONITRILE

85554-24-1
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Yield:82-07-5 95.3%

Reaction Conditions:

with sodium hydroxide in water at 100; for 8 h;Concentration;Temperature;

Steps:

2 Tons-9-formic acid synthesis
NaOH (50 g, 1.25 mol, 2.5 eq) was dissolved in 120 mL of water and then 9-cyanoperbitol (103.5 g,0.5mol, 1.0eq) was stirred to form a suspension, and then heated to 100 ° C reflux, the reaction system gradually becomes a clear solution, continueThe reaction was refluxed 8h, the reaction was completed, cooled to room temperature, ethylene glycol dimethyl ether (200mL * 2) extraction, retaining the water phase accounted for tons -9-sodium formate solution, the aqueous solution was cooled to 0 ~ 5 , then add 6mol / L dilute hydrochloric acid under stirring to adjust the pH = 1 ~ 2, with largeThe amount of solid precipitation, stirring was continued for 1h, filtered, vacuum dried at 50 ° C to give an off-white solid accounting t-9-carboxylic acid 107.8g, yield95.3%

References:

Changzhou Tianhua Pharmaceutical Co., Ltd.;Li Guangwen;Li Jianping;Ni Guocheng CN107353275, 2017, A Location in patent:Paragraph 0035; 0042; 0043; 0044; 0051; 0052

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