Pramiracetam hydrate crystal and preparation method thereof

A kind of technology of pramiracetam hydrate and monohydrate, applied in the field of pramiracetam hydrate crystal and preparation thereof

Inactive Publication Date: 2020-11-03
ZHEJIANG LANGHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, my country does not import the raw materials and preparations of this product

Method used

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  • Pramiracetam hydrate crystal and preparation method thereof
  • Pramiracetam hydrate crystal and preparation method thereof
  • Pramiracetam hydrate crystal and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0028] In an example, the preparation method includes the following steps.

[0029] Step S101, providing a solution of pramiracetam.

[0030] The solution is prepared by dissolving pramiracetam in an organic reagent. Different from the selection of tetrahydrofuran as the solvent used in the foregoing example, any one of toluene, n-heptane, methyl tert-butyl ether, n-hexane and cyclohexane is used in this application. Alternatively, a composition of tetrahydrofuran and any one of toluene, n-heptane, methyl tert-butyl ether, n-hexane and cyclohexane may also be used. For example, a mixture of tetrahydrofuran and n-hexane; or, a mixture of toluene and tetrahydrofuran; or a mixture of n-heptane and tetrahydrofuran, and the like.

[0031] Moreover, in order to improve the dissolution effect, in some examples, a temperature higher than room temperature (such as 35°C to 50°C, for example, 36°C, 39°C, 41°C, 44°C or 48°C) is selected as the dissolution temperature . Also, stir if d...

Embodiment 1

[0047] The preparation method of pramiracetam monohydrate and dihydrate crystal form comprises the following steps.

[0048] (1) Add 5g of water to a 25mL constant pressure dropping funnel and set aside.

[0049] (2) Add 30g of pramiracetam (Base) and 50mL of toluene to a 250mL four-neck flask successively at room temperature, then raise the temperature to 35-50°C under stirring, and stir for 30min until completely dissolved to form a clear solution.

[0050] (3) Control the temperature at 20-50°C, add the water in step (1) dropwise to the solution in step (2), and the dropwise addition time is about 30min-1h. After the dropwise addition, keep stirring at the same temperature for 1.5h, and then cool down Crystallize at 5-15°C for 12h.

[0051] (4) After crystallization, filter, rinse the filter cake with 15mL of toluene, and suction filter until dry; take out the filter cake and dry it in vacuum at 30-42°C for 12 hours to a moisture content of 5.0-7.0%, to obtain a white soli...

Embodiment 2

[0063] The preparation method of pramiracetam monohydrate and dihydrate crystal form comprises the following steps.

[0064] (1) Add 5g of water to a 25mL constant pressure dropping funnel and set aside.

[0065] (2) Add 30g of pramiracetam (Base) and 50mL of n-heptane to a 250mL four-necked flask successively at room temperature, then raise the temperature to 35-50°C under stirring, and stir for 30min until completely dissolved.

[0066] (3) Control the temperature at 20-50°C, add the water in step (1) dropwise to the solution in step (2), and the dropwise addition time is about 30min-1h. After the dropwise addition, keep stirring at the same temperature for 1.5h, and then cool down Crystallize at 5-15°C for 12h.

[0067] (4) After the crystallization is completed, filter, rinse the filter cake with 15 mL of n-heptane, and suction filter to dryness. The filter cake was taken out and vacuum-dried at 30-42° C. for 12 hours to a moisture content of 5.0-7.0%, and a white solid ...

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Abstract

The invention discloses a pramiracetam hydrate crystal and a preparation method thereof, and belongs to the field of medicines. The preparation method of the pramiracetam hydrate crystal comprises thefollowing steps: providing a pramiracetam solution in which a solvent is an organic reagent; dropwise adding water into the solution, cooling the solution to crystallize, and filtering the liquid; leaching the crystal by using an organic reagent and carrying out suction filtration at the same time; and drying the filter cake under a vacuum condition until the water content is 5-7% to obtain a monohydrate crystal. According to the preparation method, relatively high crystal yield and purity can be obtained.

Description

technical field [0001] The application relates to the field of medicine, in particular to a pramiracetam hydrate crystal and a preparation method thereof. Background technique [0002] Pramiracetam belongs to pyrrolidone nootropic drugs, its English name is: Pramiracetam, trade name: Piracetam, chemical name is N-[2-(N,N-diisopropyl)ethyl]-2-oxo- 1-Pyrrolidineacetamide, CAS No.: 68497-62-1. Its structural formula is as follows: Developed by the Warner-Lambert Company of the United States, it was first launched in Italy in 1993, and has been listed in Argentina, Australia, France, and Japan successively. At present, my country does not import the raw materials and preparations of this product. [0003] Alzheimer's disease is a chronic progressive disease characterized by mental decline, obvious changes in behavior and personality, and accompanied by systemic tissue and organ decline. Senile dementia includes cerebrovascular dementia, Alzheimer's dementia, mixed dementia ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/27A61P25/28
CPCC07D207/27A61P25/28C07B2200/13
Inventor 林祖峰张锦潇周灵祺孙宝丹赵海王世辉林邦平班艳
Owner ZHEJIANG LANGHUA PHARMA
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