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Preparation method of tamsulosin hydrochloride crystal form

A technology of tamsulosin crystal form and hydrochloric acid, which is applied in the preparation of sulfonamides, organic chemistry methods, organic chemistry, etc., can solve problems affecting clinical efficacy and drug quality, affecting dissolution speed and stability, and different solubility , to achieve the effect of high product purity, high yield and simple process

Pending Publication Date: 2020-12-29
北京鑫开元医药科技有限公司 +1
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Problems solved by technology

Different crystal forms may have different solubility, which may affect their dissolution rate and stability after being made into a certain dosage form, thereby affecting clinical efficacy and drug quality

Method used

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  • Preparation method of tamsulosin hydrochloride crystal form
  • Preparation method of tamsulosin hydrochloride crystal form

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preparation example Construction

[0025] The embodiment of the present invention provides a preparation method of tamsulosin hydrochloride crystal form, comprising:

[0026] Step S11, adding tamsulosin to the solvent, raising the temperature to the first temperature, and obtaining the first solution after being completely dissolved;

[0027] Step S12, adding an acid to the first solution, and obtaining a second solution after keeping warm at the first temperature;

[0028] Step S13, cooling the second solution to a second temperature, stirring and reacting to obtain a third solution;

[0029] Step S14, after filtering and drying the third solution, the crystal form of tamsulosin hydrochloride is obtained.

[0030] Further, in step S11, the solvent includes at least one of acetonitrile, ethanol, acetone and tetrahydrofuran, preferably the solvent is acetonitrile.

[0031] The first temperature is 30°C to 85°C, for example, 30°C, 31°C, 32°C, 33°C, 34°C, 35°C, 40°C, 45°C, 50°C, 60°C, 70°C, 80°C, 85°C, etc., pr...

Embodiment 1

[0041] Step S1: Add 5g of tamsulosin into the reaction flask, then add 50mL of acetonitrile, heat up to 60-70°C, and completely dissolve to obtain the first reaction solution;

[0042] Step S2: Add 7.5 g of concentrated hydrochloric acid dropwise to the above first reaction solution, and keep the reaction for 1 hour under the condition of 60-70° C. to obtain the second reaction solution;

[0043] Step S3: Slowly cool the second reaction solution to about 25°C, and then stir for 5 hours to obtain a third reaction solution;

[0044] Step S4: Filter and dry the above-mentioned third reaction solution to obtain 5.17 g of a white solid, which is the crystal form of tamsulosin hydrochloride, HPLC: 99.98%, and the yield is 95%.

[0045] The XRD pattern of tamsulosin hydrochloride crystal form is shown in figure 1 , the testing instrument is D2 Phaser X-ray powder diffractometer. The test conditions: anode target, Cu target; tube pressure 30kV, tube current 10mA; 2θ scanning range 4...

Embodiment 2

[0048] Step S1: Add 5g of tamsulosin into the reaction flask, then add 50mL of ethanol, heat up to 70-75°C, and completely dissolve to obtain the first reaction solution;

[0049] Step S2: Add 7.5 g of concentrated hydrochloric acid dropwise to the above first reaction solution, and keep warm for 1 hour under the condition of 70-75° C. to obtain the second reaction solution;

[0050] Step S3: Slowly cool the second reaction solution to about 25°C, and then stir for 5 hours to obtain a third reaction solution;

[0051] Step S4: Filter and dry the above third reaction solution to obtain 4.95 g of white solid, which is the crystal form of tamsulosin hydrochloride, HPLC: 99.89%, yield 91%.

[0052] For the XRD pattern and DSC pattern of tamsulosin hydrochloride crystal form, refer to Example 1.

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a preparation method of a tamsulosin hydrochloride crystal form, which comprises the following steps: adding tamsulosin into a solvent, conducting heating to a first temperature, and conducting complete dissolving to obtain a first solution; adding an acid into the first solution, and carrying out heat preservation reaction at a first temperature to obtain a second solution; cooling the second solution to a second temperature, and conducting stirring for reaction to obtain a third solution; and filtering thethird solution and conducting drying to obtain the tamsulosin hydrochloride crystal form. The preparation method is simple in process, high in yield, high in product purity and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a preparation method of tamsulosin hydrochloride crystal form. Background technique [0002] The chemical name of Tamsulosin Hydrochloride is 5-[(2R)-2-[[2-(2-ethoxyphenoxy)ethyl]amino]propyl]-2-methoxy Benzenesulfonamide hydrochloride; the molecular formula of tamsulosin hydrochloride is C 20 h 28 N 2 o 5 S·HCl, the molecular weight is 444.97; there is a chiral carbon atom in the molecular structure of tamsulosin hydrochloride, and the clinically used drug has its R configuration. [0003] Tamsulosin hydrochloride is a new type of long-acting α-1 adrenoceptor antagonist, developed by Japan Yamanouchi Pharmaceutical Co., Ltd., and approved by FDA in July 1992. Its trade name is Harnal (Hale). The drug can specifically inhibit the contraction of the smooth muscle of the prostate, rapidly relieve the clinical symptoms of benign prostatic hyperplasia, and has th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/36C07C311/37
CPCC07C303/36C07B2200/13C07C311/37
Inventor 昝广友曹祺于凯王永广戴信敏
Owner 北京鑫开元医药科技有限公司
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