Preparation of Azelnidipine alpha crystal form

A technique for the crystal form of azedipine, which is applied in the field of crystal form conversion of organic compounds, can solve the problems of literature or patents on the preparation method of α crystal form, and achieve the effects of good quality, easy recycling, and reduced manufacturing costs

Active Publication Date: 2009-07-22
QINGDAO HUANGHAI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are relatively few introductions to azedipine in Chinese patents and literature, and there are no literature or patents on the preparation method of α crystal form

Method used

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  • Preparation of Azelnidipine alpha crystal form
  • Preparation of Azelnidipine alpha crystal form
  • Preparation of Azelnidipine alpha crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Preparation of Azeldipine α Crystal Form

[0020] Take 20g of crude Azedipine, dissolve it in 20ml of ethyl acetate and 150ml of benzene (when dissolving, first mix the two organic solvents, and then add Azedipine), heat it in a water bath to 40°C, add 200ml of cyclohexane, 0.1 g seed crystals, cooled to 20° C. for crystallization, and the precipitated crystals were collected with a yield of 85%.

[0021] Carry out DSC analysis to the Azeldipine α crystal form prepared by the above-mentioned method and the crude product of Azeldipine, the results are as follows: figure 2 , image 3 shown. Carry out X-ray diffraction analysis to the Azeldipine α crystal form that above-mentioned method prepares, the result is as follows figure 1 shown. As can be seen from the figure, the α-crystal form of azeldipine prepared by the method of the present invention has high purity and good quality.

Embodiment 2

[0022] Example 2: Preparation of Azeldipine α Crystal Form

[0023] The water bath was heated to 45° C., and the rest was the same as in Example 1, and the final yield was 87%.

Embodiment 3

[0024] Example 3: Preparation of Azeldipine α Crystal Form

[0025] The water bath was heated to 50° C., and the rest was the same as in Example 1, and the final yield was 90%.

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Abstract

The invention discloses a preparation method of Azelnidipine of alpha crystal form, wherein, Azelnidipine of non-alpha crystal forms is completely dissolved in a two-phase organic solvent. Water-bath is heated to certain temperature and alkane and seed crystal are added into the solution under a stirring condition. A crystal is separated out by cooling and a separated crystal product is collected, namely the Azelnidipine of alpha crystal form. The two-phase organic solvent comprises two components: low boiling point esters and benzene or derivatives of benzene, with a volume ratio of 1 to 3:15. The preparation method has one-time yield up to 85 percent to 90 percent, purity of more than 99.5 percent as well as good appearance and quality. The preparation method has easily recycled organic solvent, is beneficial to environmental protection, reduces loss in Azelnidipine and/or waste in the organic solvent, greatly reduces the production costs of products and has prospect of large-scale industrialized production.

Description

technical field [0001] The invention relates to a method for converting crystal forms of organic compounds, in particular to a method for preparing α-crystal forms of azedipine. Background technique [0002] Azhedipine is a dihydropyridine calcium ion antagonist jointly developed by Japan Sankyo (SANKYO) Co., Ltd. and Japan Ube Industries Co., Ltd. It was first listed in Japan in 2003. The trade name is Calblock, and there are 8mg and 16mg. Two specifications for the treatment of essential hypertension. Oral administration of Azedipine once a day can control blood pressure stably and 24 hours a day, increase cardiac output, have little effect on heart rhythm, do not cause reflex tachycardia, and can slightly reduce heart rhythm after long-term medication, while other pyridines Antagonists have no such effect, and are especially suitable for long-term treatment of hypertensive patients with potential cardiac ischemia. [0003] Azedipine has two crystal forms, the α crystal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12A61P9/12
Inventor 赵明媚祝少良隋宇
Owner QINGDAO HUANGHAI PHARM CO LTD
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