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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 hydrochloride in ethanol or methanol , due to the inherent physical and chemical properties of quinine hydrochloride, it is often difficult to obtain qualified quinine hydrochloride crystals only by concentrating crystallization or adding water or organic solvents to filter crystallization, etc.

Method used

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

Examples

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Effect test

Embodiment 1

[0031] (1) Preparation of quinine: quinine sulfate and water are mixed in a mass ratio of 1: 40, then the pH value of the aforementioned solution is adjusted to 4 with dilute hydrochloric acid of 1mol / L, so that quinine sulfate is dissolved; then heated to 60 ℃, under the condition of stirring, adjust the pH value of the solution to 10 with a mass percentage of 5% sodium hydroxide solution, and then stir for at least 1 hour. After the stirring is completed, cool down, filter out the precipitate quinine, and wash the precipitate with water until it is washed out The pH value of the aqueous solution was 7, and the quinine was dried at 60° C. for 4 hours after filtering to obtain quinine.

[0032] (2) Preparation of quinine hydrochloride: Weigh 3.24g of quinine in a 100mL round bottom flask, add 22mL of methanol and stir to dissolve at room temperature, slowly add about 0.91mL of concentrated hydrochloric acid with a concentration of 36% by mass percentage, under airtight conditio...

Embodiment 2

[0035] (1) Preparation of quinine: quinine sulfate and water are mixed in a mass ratio of 1: 45, then the pH value of the aforementioned solution is adjusted to 4 with 1mol / L dilute hydrochloric acid, so that quinine sulfate is dissolved; then heated to 60 ℃, under the condition of stirring, adjust the pH value of the solution to 10 with a mass percentage of 5% sodium hydroxide solution, and then stir for at least 1 hour. After the stirring is completed, cool, filter out the precipitate quinine, and wash the precipitate with water to the pH value It was 8, and 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 in 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%, and keep the The reaction was stirred for 25 min. Concentr...

Embodiment 3

[0039] (1) Preparation of quinine: quinine sulfate and water are mixed in a mass ratio of 1:50, then the pH value of the aforementioned solution is adjusted to 4 with dilute hydrochloric acid of 1mol / L, so that quinine sulfate is dissolved; then heated to 60 ℃, under the condition of stirring, adjust the pH value of the solution to 10 with a mass percentage of 5% sodium hydroxide solution, and then stir for at least 1 hour. After the stirring is completed, cool down, filter out the precipitate quinine, wash the precipitate with water until it is filtered out The pH value of the aqueous solution is 7.5, and the precipitated quinine is filtered out and dried at 70° C. for 3 hours to obtain quinine.

[0040] (2) Preparation of quinine hydrochloride: Weigh 3.24g of quinine in a 100mL round bottom flask, add 24mL of 1-propanol and stir to dissolve at room temperature, slowly add about 0.9mL of concentrated hydrochloric acid with a mass percentage concentration of 36%, and seal the f...

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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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