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Novel crystal form of pidotimod and preparation method of novel crystal form

A technology of pidotimod and crystal form, applied in the field of pharmaceutical compounds, can solve the problems of impractical preparation method, limit industrialized large-scale production and the like, and achieve the effect of promoting crystal transformation, easy industrialized large-scale production, and high stability.

Inactive Publication Date: 2017-11-10
BEIJING JINCHENG TAIER PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent uses the method of natural volatilization of solvents to prepare the new crystal form of pidotimod, which limits industrial production and the preparation method is not practical

Method used

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  • Novel crystal form of pidotimod and preparation method of novel crystal form
  • Novel crystal form of pidotimod and preparation method of novel crystal form
  • Novel crystal form of pidotimod and preparation method of novel crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 100ml of purified water and 300ml of acetone into a three-necked flask at room temperature, and then add 50.0g of pidotimod to form a suspension; stir at room temperature for 15 hours at a stirring speed of 120 rpm, then lower the temperature to 9°C and stir for 24 hours. The stirring speed was 80 rpm, and then heated to room temperature and stirred for 3 hours, and the stirring speed was 40 rpm; then suction filtration, and the obtained solid was dried at a temperature of 25 °C and a vacuum of -0.09 MPa for 10 hours to obtain The new crystal form of Domod is 43.9g, yield: 87.8%, purity: 99.85%.

Embodiment 2

[0032] Add 100ml of purified water and 100ml of acetone into a three-necked flask at room temperature, then add 50.0g of pidotimod to form a suspension, stir at room temperature for 24 hours at a stirring speed of 180 rpm, then cool down to 5°C and stir for 20 hours. The stirring speed was 60 rpm, and then heated to room temperature and stirred for 5 hours, and the stirring speed was 30 rpm; then suction filtration, and the obtained solid was dried at a temperature of 35 °C and a vacuum of -0.07 MPa for 12 hours to obtain 44.2 g of the new crystal form of Domod, yield: 88.4%, purity: 99.80%.

Embodiment 3

[0034] Add 100ml of purified water and 500ml of tetrahydrofuran into a three-necked flask at room temperature, then add 50.0g of pidotimod to form a suspension, stir at room temperature for 10 hours at a stirring speed of 150 rpm, then lower the temperature to 2°C and stir for 16 hours. The stirring speed was 70 rpm, and then heated to room temperature and stirred for 4 hours at a stirring speed of 35 rpm; then suction filtered, and the obtained solid was dried at a temperature of 40°C and a vacuum of -0.05MPa for 15 hours to obtain The new crystal form of Domod is 43.4g, yield: 86.8%, purity: 99.82%.

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Abstract

The invention belongs to the technical field of drug compounds, and particularly relates to a novel crystal form of pidotimod and a preparation method of the novel crystal form. An X-ray powder diffraction pattern of the novel crystal form of pidotimod has characteristic peaks when the reflection angle 2theta is 8.54 degrees plus / minus 0.2 degrees, 10.28 degrees plus / minus 0.2 degrees, 11.52 degrees plus / minus 0.2 degrees, 13.08 degrees plus / minus 0.2 degrees, 15.43 degrees plus / minus 0.2 degrees, 17.23 degrees plus / minus 0.2 degrees, 19.30 degrees plus / minus 0.2 degrees, 19.80 degrees plus / minus 0.2 degrees, 20.70 degrees plus / minus 0.2 degrees, 21.45 degrees plus / minus 0.2 degrees, 23.90 degrees plus / minus 0.2 degrees, 27.77 degrees plus / minus 0.2 degrees and 28.36 degrees plus / minus 0.2 degrees. The preparation method of the novel crystal form comprises the steps that pidotimod is added to an organic solvent and water mixed solution, a suspension is formed, stirred at room temperature, cooled and stirred again, heated to the room temperature and stirred again and subjected to suction filtration, a product is dried in vacuum, and the novel crystal form of pidotimod is obtained. The novel crystal form of pidotimod is high in stability and easy to produce industrially.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical compounds, and in particular relates to a new crystal form of pidotimod and a preparation method thereof. Background technique [0002] The chemical name of pidotimod is (R)-3-[(S)-(5-oxo-2-pyrrolidinyl) carboxyl]-tetrahydrothiazole-4-carboxylic acid, also known as Primo, Puleyi , Lin Kemiao, is the only immune enhancer with oral biological activity, which can promote both non-specific immune response and specific immune response. In the late 1980s, it was successfully synthesized by the Italian Poli industrialachimica S.P.A chemical company, and it was approved for marketing in 1993. The chemical structural formula is as follows: [0003] [0004] US Patent No. 4,839,387 discloses a process synthesis route of pidotimod, which uses L-4-thiazolidine formic acid and L-pyroglutamyl chloride to react under the action of sodium hydroxide to obtain pidotimod. US Patent No. 5,110,936 disclos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/078
CPCC07K5/06139C07B2200/13
Inventor 孟宾孙滨许蕾马庆双王晓光南红燕张彤
Owner BEIJING JINCHENG TAIER PHARMA CO LTD
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