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 crystallization process is large, the pressure on environmental protection is high, and the cost is high, which is not conducive to industrial production.

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

Embodiment 1

[0044] Preparation of minodronic acid crystal form II

[0045] Add 2g of minodronic acid crude product and 6ml of 6mol / L hydrochloric acid into the three-neck flask, raise the temperature to 60°C, stir to completely dissolve, slowly add methanol dropwise, and keep the reflux state, stop adding methanol dropwise when there is a little turbidity, and cool down Stir at 0°C for 2 hours, let cool to crystallize, filter, and blow dry at 80°C to obtain 1.72 g of Form II sample. Its X-ray diffraction pattern is shown in image 3 , see the infrared spectrum Figure 4 .

Embodiment 2

[0047] Minodronic Acid Form II Tablets

[0048] Tablet prescription:

[0049] Name of raw material

Dosage

Minodronic acid crystalline form II

1.0g

microcrystalline cellulose

36.0g

lactose

66.0g

Crospovidone

6.0g

Magnesium stearate

1.0g

water

about 40ml

Made into 1000 pieces

[0050] Coating Solution Prescription:

[0051] Name of raw material

Dosage

Opadry 81W680000

36.0g

water

200ml

[0052] Tablet core preparation process:

[0053] Pass the raw and auxiliary materials through 80-mesh sieves for later use; mix the main ingredient with crospovidone, microcrystalline cellulose, and lactose evenly in equal increments; use water as a wetting agent to make soft materials from the above-mentioned mixed fine powder, and pass through Granulate with a 24-mesh sieve, dry at 60°C for about 2 hours, control the water content of the g...

Embodiment 3

[0057] Minodronic Acid Form II Capsules

[0058] prescription:

[0059] Name of raw material

Dosage

Minodronic acid crystalline form II

1.0g

starch

36.0g

lactose

66.0g

Magnesium stearate

1.0g

water

about 40ml

Make 1000 capsules

[0060] Preparation Process:

[0061] Pass the raw and auxiliary materials through 80-mesh sieve for later use; mix the main ingredient, starch, and lactose evenly in equal increments; use water as a wetting agent to make soft materials from the mixed fine powder, granulate through a 24-mesh sieve, and dry at 60°C About 2 hours, control the water content of the granules to ≤3%, sieve the granules with 24 mesh, and mix well; take the above granules, add the prescribed amount of magnesium stearate, mix well, measure the content of intermediates, fill in No. 4 capsules, and you are done. .

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PUM

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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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