A kind of minodronic acid crystal form ii and preparation method thereof

A technology of minodronic acid and crystal form, applied in the field of drug synthesis, can solve the problems of poor solubility of minodronic acid crystal form I, unfavorable industrial production, low bioavailability and the like, and achieves less solvent usage, low cost, Prepare simple effects

Active Publication Date: 2011-12-07
广东宏远集团药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, minodronic acid crystal form I has disadvantages such as poor solubility and low bioavailability, and the amount of solvent used in the c

Method used

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  • A kind of minodronic acid crystal form ii and preparation method thereof
  • A kind of minodronic acid crystal form ii and preparation method thereof
  • A kind of minodronic acid crystal form ii and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0043] Example 1

[0044] Preparation of minodronic acid crystal form II

[0045] Add 2g of crude minodronic acid and 6ml of 6mol / L hydrochloric acid into a three-necked flask, heat up to 60℃, stir to dissolve completely, slowly add methanol dropwise, and keep the reflux state, stop adding methanol when there is a slight turbidity, and cool down Stir at 0°C for 2h, leave to cool to crystallize, filter, and blow dry at 80°C to obtain 1.72g of crystal form II sample. See the X-ray diffraction pattern image 3 , See the infrared spectrum Figure 4 .

Example Embodiment

[0046] Example 2

[0047] Minodronic acid crystal form II tablets

[0048] Tablet core prescription:

[0049] Name of raw materials

[0050] Coating liquid prescription:

[0051] Name of raw materials

[0052] Chip preparation process:

[0053] The raw and auxiliary materials were passed through an 80-mesh sieve for use; the main drug, crospovidone, microcrystalline cellulose, and lactose were mixed uniformly in equal increments; the above-mentioned mixed fine powder was made into soft material with water as a wetting agent. Granulate with 24 mesh sieve, dry at 60°C for about 2 hours, control the moisture content of the granules to be ≤3%, size the granules on a 24 mesh sieve, and mix well; take the above granules, add the prescribed amount of magnesium stearate, mix well, and measure the intermediate content , Use the 6.5mm diameter shallow concave punching sheet, the hardness is controlled at 5~10kg / mm 2 .

[0054] Coating process:

[0055] Under stirring, slowly add the prescri...

Example Embodiment

[0056] Example 3

[0057] Minodronic acid crystal form II capsules

[0058] prescription:

[0059] Name of raw materials

[0060] Preparation Process:

[0061] Separate the raw and auxiliary materials through an 80-mesh sieve for use; mix the main drug with starch and lactose in equal increments; use water as a wetting agent to make the above-mentioned mixed powder into a soft material, granulate through a 24-mesh sieve, and dry at 60°C About 2 hours, control the moisture content of the granules ≤3%, size the granules through a 24-mesh sieve, and mix them; take the above granules, add the prescribed amount of magnesium stearate, mix well, measure the intermediate content, and fill the No. 4 capsules. .

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Abstract

The invention relates to the field of synthesis of medicines, in particular to a minodronate crystalform II and a preparation method thereof. The minodronate crystalform II is characterized in that an X-ray powder diffraction pattern has characteristic peaks when a reflection angle 2theta is close to 10.32, 11.16, 13.14, 15.02, 15.72, 17.44, 20.28, 20.72, 21.46, 22.30, 23.48, 25.64, 26.48, 28.80, 30.14, 32.30, 34.58, 35.50 and 36.34. The minodronate crystalform II has high solubility and dissolution rate.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a crystal form II of minodronic acid and a preparation method thereof. Background technique [0002] Minodronic Acid (Minodronic Acid), its chemical name is: [1-hydroxyl-2-(imidazo[1,2-a]pyridin-3-yl)ethylidene]bisphosphonic acid monohydrate, its anti The bone resorption activity is 100-1000 times higher than that of pamidronate sodium, and it can antagonize the osteolysis caused by myeloma and tumor. It is clinically used for the treatment of osteoporosis. [0003] The crystallization methods of minodronic acid reported in the current literature are all carried out in a water and methanol system. According to the preparation method reported by the patent US4990503, the inventor obtained the known crystal form I of minodronic acid through the recrystallization method using water and methanol, and the powder X-ray diffraction of the crystal form figure 2 θ near 9.60, 10.40, 12.18, ...

Claims

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Application Information

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IPC IPC(8): C07F9/6561A61K31/675A61P19/10
Inventor 何广卫李丰刘为中王银虎刘伟
Owner 广东宏远集团药业有限公司
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