Hydroxyl amyl benzoate potassium crystal and preparation method thereof

A technology of hydroxyamylbenzene and potassium formate, applied in the field of medicine, can solve problems such as being unsuitable for large-scale production, high risk, unstable to humidity and the like

Inactive Publication Date: 2013-05-22
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned recrystallization solvents are highly toxic, such as chloroform, or have a low boiling point and high risk, such as ether, which are not suitable for large-scale production
In addition, Chinese patent application CN1523003A records that potassium hydroxyamylbenzoate has strong hygroscopicity, is unstable to humidity, and is easy to decompose when placed in an ordinary environment.

Method used

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  • Hydroxyl amyl benzoate potassium crystal and preparation method thereof
  • Hydroxyl amyl benzoate potassium crystal and preparation method thereof
  • Hydroxyl amyl benzoate potassium crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Preparation of Potassium Hydroxypentyl Benzoate Crystal III

[0034] Add 10 g of crude potassium hydroxyamyl benzoate into 50 mL of isopropyl ether, heat to reflux to dissolve, cool to room temperature, stir and crystallize for 1 h, filter and dry to obtain 9.3 g of white crystals. The obtained crystal sample is subjected to powder X-ray diffraction, and the obtained collection of illustrative plates is shown in the attached figure 1 , and the spectral data are shown in Table 1.

Embodiment 2

[0035] Embodiment 2: Preparation of Potassium Hydroxypentyl Benzoate Crystal III

[0036] Add 10 g of crude potassium hydroxyamyl benzoate into 100 mL of ethyl acetate, heat to dissolve, cool to 5°C, stir and crystallize for 2 h, filter and dry to obtain 8.5 g of white crystals. The obtained crystal sample is subjected to powder X-ray diffraction, and the obtained collection of illustrative plates is shown in the attached image 3 , and the spectral data are shown in Table 1.

Embodiment 3

[0037] Embodiment 3: Preparation of Potassium Hydroxypentyl Benzoate Crystal III

[0038] Add 10 g of crude potassium hydroxyamyl benzoate into 200 mL of tert-methyl ether, heat to reflux to dissolve, cool to 0°C, stir and crystallize for 2 h, filter and dry to obtain 8.2 g of white crystals. The obtained crystal sample is subjected to powder X-ray diffraction, and the obtained collection of illustrative plates is shown in the attached Figure 5 , and the spectral data are shown in Table 1.

[0039] Table 1 Powder X-ray Diffraction Characteristic Peak Data of Crystal Samples of Examples 1~3

[0040] .

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PUM

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Abstract

The invention discloses a hydroxyl amyl benzoate potassium crystal and a preparation method thereof. The powder of the hydroxyl amyl benzoate potassium crystal disclosed by the invention has characteristic peaks under X-ray diffraction at 2theta, namely 7.0+ / -0.2 degrees and 20.9+ / -0.2 degrees. The hydroxyl amyl benzoate potassium crystal disclosed by the invention is stable in quality, stable in crystal form and more suitable for storage and use as a crude drug.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to potassium hydroxyamylbenzoate crystals and a preparation method thereof. Background technique [0002] Cerebrovascular disease (stroke) is a disease caused by blockage or rupture of cerebral blood vessels that blocks blood flow in the brain. It is divided into ischemic stroke and hemorrhagic stroke. According to reports, the results of sample surveys of urban and rural populations in my country show that the annual incidence rates are 219 / 100,000 and 185 / 100,000, respectively, and the mortality rates are 116 / 100,000 and 141.8 / 100,000, and they tend to be younger. There are about 1.5-2 million new stroke patients in my country every year, of which ischemic stroke accounts for about 60-80% of stroke cases. In 1992, among the causes of death of urban and rural population in my country, stroke ranked second, accounting for 21.13% and 16.18% of the total number of deaths...

Claims

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Application Information

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IPC IPC(8): C07C51/43C07C65/01A61K31/192A61P9/10
CPCC07C51/43C07C65/01
Inventor 郑利刚尹跳刘洋马玉秀杨占坤郭明东郭晓伟李海波齐珊张頔
Owner CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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