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ChemicalBook CAS DataBase List Diacetonefructose

Diacetonefructose synthesis

9synthesis methods
-

Yield:20880-92-6 90.7%

Reaction Conditions:

with ammonia in dichloromethane at 20 - 30;Temperature;Solvent;

Steps:

4
The pale yellow oil obtained in the next step was dissolved in 300 ml of dichloroethane, 20-30 ° C was passed through ammonia for 5-7 hours,The resulting solid was filtered and the filter cake was rinsed with 30 ml of dichloroethane. The organic phases were combined and 18.5 g of a 50% sodium hydroxide solution was added at 20 ° C and stirred at 20-30 ° C for 3 hours. The filter cake was washed with 30 ml of dichloroethane Leaching. The obtained filter cake was dissolved in 60 ml of water at a temperature of not more than 30 ° C and adjusted to pH 6-7 ° C with hydrochloric acid for 2 hours. The resulting solid was dried at 60 ° C or lower. The crude product was 30 g, yield 76.7%. The crude product was heated to 55 ° C with 33 ml of 95% ethanol, dissolved in 0.5 g of activated charcoal, and then cooled to below 10 ° C for 2 hours. The mixture was filtered and dried at 50 ° C to obtain 27 g of topiramate, 90.0% Phase purity 99.91%. The procedure was repeated with 30 ml of 95% ethanol to give topiramate 24.5 g yield 90.7% and liquid phase purity 99.95%.

References:

Shanxi Da Sheng Pharmaceutical Technology Co., Ltd.;Xue Chaoyun;Yang Gangli CN106632530, 2017, A Location in patent:Paragraph 0009; 0037; 0043; 0044; 0048

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