- Preparation method of medicine for treating chronic hyperuricemia
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The invention discloses a preparation method of a medicine for treating chronic hyperuricemia. The method comprises the following steps: using methyl 2-cyanoisonicotinate and 4-cyanopyridine as initial raw materials, and carrying out hydrazinolysis reaction, condensation reaction, cyclization reaction and purification to obtain topiroxostat. On one hand, by using a hydrochloric acid alcohol solution, the energy consumption of the process is reduced, and the problem of poor safety is improved; and on the other hand, topiroxostat hydrochloride is refined and concentrated in alcohol water and then subjected to a salt dissolving process, so that the solubility of the topiroxostat in an alkaline solution is increased, the problem that chloride exceeds the standard is preliminarily solved, the salt dissolving process is more thorough, and the reaction proceeding degree is increased. Finally, in the purification process, the amount of chlorides in the product is further reduced by a method of hot melting the crude product in alcohol water, and the product quality is ensured; and the purity of the product is improved by selecting a purification solvent.
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- Preparation method of topiroxostat
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The invention provides a preparation method of topiroxostat. The preparation method comprises the steps that 2-cyano methyl isonicotinate is used as raw materials; hydrazinolysis is performed at -10 DEG C to -20 DEG C to obtain an intermediate; the intermediate and 4-cyanopyridine react under the conditions with sodium ethoxide and the pH being 4 to 6 to obtain the topiroxostat. The preparation method has the advantages that the 2-cyano methyl isonicotinate is used as a starting material; the 2-cyano methyl isonicotinate and hydrazine hydrate take condensation reaction at low temperature to prepare the intermediate; the intermediate and the 4-cyanopyridine are subjected to condensation and loop closing under the acid condition with sodium ethoxide to prepare the topiroxostat. The raw materials can be easily obtained; the reaction conditions are mild and are easy to control; a reagent with high toxicity is not used in the reaction process; the released toxic substances are few; the sidereaction products are few; the reaction safety is high; the pollution is small; the obtained purity is high; the preparation method is suitable for industrial production.
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- One-pot method for synthesizing Topiroxostat
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The invention discloses a one-pot method for synthesizing Topiroxostat. The one-pot method comprises the following steps: dissolving 2-cyano methyl isonicotinate into a solvent, reacting with hydrazine hydrate to generate an intermediate 2-cyanoisoniazide, then adding alkali for reaction in the same reactor, then adding 4-cyanopyridine to form a ring, and finally purifying to obtain the Topiroxostat. The one-pot method is short in technological process, simple in operation, high in raw material utilization rate and low in production cost, and has higher production and practical value.
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Paragraph 0019; 0020
(2017/01/02)
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