Preparation method of quinine hydrochloride

A technology of quinine hydrochloride and quinine sulfate, which is applied in the fields of separation and purification and derivative preparation, can solve the problems that it is not easy and difficult to obtain quinine hydrochloride crystallization, precipitation and filtration is cumbersome, and achieves low cost and is beneficial to scaled production and preparation. The effect of simple and convenient process operation

Inactive Publication Date: 2011-01-19
JINAN UNIVERSITY
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  • Description
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Problems solved by technology

These methods seem to be simple, but in fact they are not easy. To use toxic barium chloride, barium chloride must be excessive, and the formed barium sulfate precipitate is close to colloid, and the precipitation and filtration are more cumbersome; after generating quinine hydrochlori

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  • Preparation method of quinine hydrochloride
  • Preparation method of quinine hydrochloride
  • Preparation method of quinine hydrochloride

Examples

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[0030] Example 1

[0031] (1) Preparation of quinine: mix quinine sulfate and water at a mass ratio of 1:40, then adjust the pH of the aforementioned solution to 4 with 1 mol / L dilute hydrochloric acid to dissolve quinine sulfate; then heat to 60 ℃, under stirring conditions, adjust the pH of the solution to 10 with 5% by mass sodium hydroxide solution, stir for at least 1 hour, after stirring, cool, filter out the precipitate quinine, wash the precipitate with water until it is washed out The pH of the aqueous solution is 7, and the quinine after filtering the water is dried at 60°C for 4 hours to obtain quinine.

[0032] (2) Preparation of quinine hydrochloride: Weigh 3.24g of quinine into a 100mL round bottom flask, add 22mL of methanol to dissolve at room temperature, and slowly add about 0.91mL of concentrated hydrochloric acid with a concentration of 36% by mass. The reaction was stirred for 20 min. Concentrate under reduced pressure until the solids in the bottle are compl...

Example Embodiment

[0034] Example 2

[0035] (1) Preparation of quinine: mix quinine sulfate and water at a mass ratio of 1:45, then adjust the pH of the aforementioned solution to 4 with 1 mol / L dilute hydrochloric acid to dissolve quinine sulfate; then heat to 60 ℃, under stirring conditions, adjust the pH of the solution to 10 with 5% by mass sodium hydroxide solution, stir for at least 1 hour, after stirring, cool, filter out the precipitate quinine, wash the precipitate to pH value It was 8, the precipitated quinine was filtered and dried at 65°C for 4 hours to obtain quinine.

[0036] (2) Preparation of quinine hydrochloride: Weigh 3.24g of quinine into a 100mL round bottom flask, add 18mL of ethanol alcohol and stir to dissolve at room temperature, slowly add about 0.91mL of concentrated hydrochloric acid with a mass percentage concentration of 36% in a closed condition The reaction was stirred for 25 min. Concentrate under reduced pressure until the solid matter appears in the bottle, add 2...

Example Embodiment

[0038] Example 3

[0039] (1) Preparation of quinine: mix quinine sulfate and water at a mass ratio of 1:50, then adjust the pH of the aforementioned solution to 4 with 1 mol / L dilute hydrochloric acid to dissolve quinine sulfate; then heat to 60 ℃, under stirring conditions, adjust the pH of the solution to 10 with 5% by mass sodium hydroxide solution, stir for at least 1 hour, after stirring, cool, filter the precipitate quinine, wash the precipitate with water to filter out The pH of the aqueous solution was 7.5, and the filtered precipitate quinine was dried at 70°C for 3 hours to obtain quinine.

[0040] (2) Preparation of quinine monohydrochloride: Weigh 3.24g quinine into a 100mL round bottom flask, add 24mL 1-propanol to dissolve at room temperature, and slowly add about 0.9mL of concentrated hydrochloric acid with a mass percentage concentration of 36%, and airtight Under the circumstances, the reaction was stirred for 30 min. After concentrating and recovering the solve...

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Abstract

The invention discloses a preparation method of quinine hydrochloride. The method of the invention comprises the following steps: transforming quinine sulfate to quinine, then dispersing the quinine into a dispersing agent, adding hydrochloric acid or introducing hydrogen chloride gas to react, and the quinine hydrochloride is obtained through the method of crystallization. Only the common acids and bases, and the common solvents with low toxicity and low price are used in the method of the invention, and the chemical reagents with high toxicity are not used. The method has high yield which is same as or close to the theoretical yield, and the yield can reach 110 to 115% measured in terms of the quinine. Further, the method is environmentally friendly. The whole preparation process of theinvention has simple and convenient operation and low cost, and is beneficial to the production amplification.

Description

technical field [0001] The invention particularly relates to a preparation method of quinine monohydrochloride and quinine dihydrochloride, which belongs to the field of separation, purification and derivative preparation. Background technique [0002] According to the latest report of the World Health Organization, malaria is an infectious disease with a clear upward trend in the world except AIDS. It is a communicable disease in tropical and subtropical regions, endangering the health of two billion people; falciparum malaria causes 4 Infecting more than 100 million people and dying about 3 million people (mostly children), it has become the number one killer of human life and health in Africa. [0003] Quinine in cinchona alkaloids is the earliest antimalarial drug discovered and used by humans, and quinine monomer was isolated and purified in the early 20th century. Although there are many antimalarial drugs at present, cinchona alkaloids are still the most common antim...

Claims

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Application Information

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IPC IPC(8): C07D453/04
Inventor 蒲含林吴毅武姜华陈蓉蓉
Owner JINAN UNIVERSITY
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