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Crystal form of doxofylline and preparation method of crystal form of doxofylline

A technology of doxofylline and crystal form, applied in the field of drug synthesis, can solve the problems of low solubility of doxofylline and low purity of doxofylline, and achieve the effect of high water solubility

Pending Publication Date: 2020-11-24
开封康诺药业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the dosage form of doxofylline is mainly injection, and the solubility of doxofylline in water is not high, according to the Chinese Pharmacopoeia, doxofylline belongs to slightly soluble; and, existing doxofylline purity is not high, usually 95-98%

Method used

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  • Crystal form of doxofylline and preparation method of crystal form of doxofylline
  • Crystal form of doxofylline and preparation method of crystal form of doxofylline
  • Crystal form of doxofylline and preparation method of crystal form of doxofylline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 20.0g of doxofylline, 80ml of toluene, 20ml of absolute ethanol, and 10ml of purified water into the three-neck flask, heat up to 75°C, stir to dissolve, then cool down to 5°C, crystallize for 2 hours, filter, and put the filter cake at 80°C Vacuum drying gave 13.7 g of white crystalline powder with a yield of 68.5% and a purity of 99.8%.

Embodiment 2

[0021] Add 100.0g of doxofylline, 200ml of toluene, 400ml of absolute ethanol, and 50ml of purified water into the three-neck flask, heat up to 75°C, stir to dissolve, then cool down to 5°C, crystallize for 2 hours, filter, and put the filter cake at 80°C Vacuum drying gave 83.7 g of white crystalline powder with a yield of 83.7% and a purity of 99.7%.

Embodiment 3

[0023] Add 20.0g of doxofylline, 100ml of toluene, 100ml of absolute ethanol, and 10ml of purified water into the three-necked flask, heat up to 70°C, stir to dissolve, then cool down to 0°C, crystallize for 2 hours, filter, and put the filter cake at 80°C Vacuum drying gave 17.0 g of white crystalline powder with a yield of 85.0% and a purity of 99.7%.

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Abstract

The invention discloses a crystal form of doxofylline. The crystal form shows characteristic peaks at 8.60 + / -0.1 degrees, 11.31 + / -0.1 degrees, 15.02 + / -0.1 degrees, 16.91 + / -0.1 degrees, 17.32 + / -0.1 degrees and 18.63 + / -0.1 degrees according to an X-ray diffraction spectrum expressed by a 2 theta angle; the differential scanning calorimetry determines that an absorption single peak exists at 143.3 DEG C, and the crystal form is formed by recrystallizing doxofylline with a mixed solvent of methylbenzene, absolute ethyl alcohol and water. The invention provides a novel crystal form of doxofylline, the novel crystal form has high water solubility, the API purity can reach 99% or above and is close to 100%, almost no impurity is detected, and the novel crystal form is suitable for injectiondosage forms.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a crystal form of doxofylline and a preparation method thereof. Background technique [0002] Doxofylline (Doxofylline), the chemical name is 7-[(1,3-dioxol-2-yl)methyl]-1,3-dimethyl-3,7-dihydro-lH- Purine-2,6-dione, its structural formula is shown in formula 1. Doxofylline was launched in Italy in 1988 under the trade name Ansimar. Doxofylline has a strong anti-asthma effect and is a new drug for dilating the bronchi. It is suitable for chronic obstructive pulmonary disease (COPD), bronchial asthma, chronic asthmatic bronchitis and other dyspnea caused by bronchospasm. [0003] [0004] When the crystal form of the drug is different, its physicochemical properties will change significantly. Because the dosage form of doxofylline is mainly injection, and the solubility of doxofylline in water is not high, according to the Chinese Pharmacopoeia, doxofylline belongs to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/08A61K31/522A61P11/06A61K9/08
CPCC07D473/08A61P11/06A61K9/08A61K9/0019C07B2200/13
Inventor 王康林周多玲张文腾孙跃军杨甲旺谌宗永
Owner 开封康诺药业有限公司