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Olopatadine hydrochloride alpha methyl compound B crystal form and preparation method and application thereof

A technology for olopatadine hydrochloride and compound, which is applied in the field of olopatadine hydrochloride alpha methyl compound B crystal form and its preparation field, can solve problems such as difference in bioavailability, difficulty in dispersion, unfavorable industrial production and the like, and achieve rapid effect , release the effect of good performance

Pending Publication Date: 2022-05-13
唯智医药科技(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the same drug has different crystal forms, and its bioavailability may also be different. In addition, its stability, solubility, fluidity, and compressibility may also be different, which will affect the efficacy of the drug.
Chinese patent CN111808063A discloses a preparation method of olopatadine hydrochloride α-methyl compound, but the corresponding crystalline form solubility of the obtained olopatadine hydrochloride α-methyl compound product is relatively poor, and the solid is not easy to disperse. When it takes a long time to stir and disperse, it will further cause difficulty in dispersing during formal production, which is not conducive to future industrial production

Method used

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  • Olopatadine hydrochloride alpha methyl compound B crystal form and preparation method and application thereof
  • Olopatadine hydrochloride alpha methyl compound B crystal form and preparation method and application thereof
  • Olopatadine hydrochloride alpha methyl compound B crystal form and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0032] Preparation of olopatadine hydrochloride α-methyl compound B crystal form

[0033] Add 10.00 g of olopatadine hydrochloride α-methyl compound into the Soxhlet extraction tube, add 80 mL of acetone into the extraction bottle, stir and raise the temperature to reflux for extraction. When there is no obvious solid in the Soxhlet extraction tube, stop heating and remove the acetone. Replace the extraction tube with a distillation device and carry out normal pressure distillation. When solids are obviously separated out in the solution, stop the distillation, keep warm and reflux for 1h, and cool down naturally for crystallization. After filtering and drying, collect the solid precipitation to obtain 5.61g of olopatadine hydrochloride. α-methyl compound B crystal form, see image 3 ; The corresponding filtrate (mother liquor) is collected and preserved for subsequent use.

[0034] The obtained XRPD pattern of Form B has diffraction peaks at 2θ=15.9°, 17.0°, 18.6°, 23.0°, 24....

Embodiment 2

[0036] Preparation of olopatadine hydrochloride α-methyl compound B crystal form

[0037] Add 10.00 g of olopatadine hydrochloride α-methyl compound into the Soxhlet extraction tube, add 20 mL of the mother liquor obtained in Example 1 into the extraction bottle, then add 80 mL of acetone, stir and heat up to reflux for extraction, and wait for Soxhlet extraction When there is no obvious solid in the tube, stop heating, remove the Soxhlet extraction tube, and replace it with a distillation device for atmospheric distillation. When solids are obviously precipitated in the solution, stop the distillation, keep warm and reflux for 1 hour, cool down naturally for crystallization, and filter and dry. 7.83 g of olopatadine hydrochloride α-methyl compound B crystal form was obtained. It shows that this method can be used for repeated recovery and extraction, which is beneficial to save costs.

Embodiment 3

[0039] Preparation of olopatadine hydrochloride α-methyl compound B crystal form

[0040] Add 10.00 g of olopatadine hydrochloride α-methyl compound into the Soxhlet extraction tube, add 100 mL of methanol into the extraction bottle, stir and heat up to reflux for extraction, and maintain a strong reflux state. When there is no obvious solid in the Soxhlet extraction tube, Stop heating, remove the Soxhlet extraction tube, and replace it with a distillation device for atmospheric distillation. When solids are clearly precipitated in the solution, stop the distillation, keep warm and reflux for 1 hour, cool down naturally to crystallize, and filter and dry to obtain 4.77g of olotaxa hydrochloride. Determine the crystal form of α-methyl compound B.

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Abstract

The invention discloses an olopatadine hydrochloride alpha methyl compound B crystal form as well as a preparation method and application thereof, and belongs to the technical field of medicines. The invention develops and prepares an olopatadine hydrochloride alpha methyl compound B crystal form, the XRPD pattern of the olopatadine hydrochloride alpha methyl compound B crystal form contains the following diffraction characteristic peaks: the diffraction angles 2theta are 15.9, 17.0, 18.6, 23.0, 24.1, 26.1 and 26.7, and the error range of each characteristic peak 2theta is + / -0.2. The olopatadine hydrochloride alpha methyl compound B crystal form is obviously improved in the aspects of drug release performance, solubility and the like, the bioavailability is improved, and the pharmaceutical prospect is wide.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to crystal form B of olopatadine hydrochloride α-methyl compound and a preparation method and application thereof. Background technique [0002] Olopatadine hydrochloride α-methyl compound has a very good effect in the treatment of skin itching and mosquito bites. However, the same drug has different crystal forms, and its bioavailability may also be different. In addition, its stability, solubility, fluidity, and compressibility may also be different, which will affect the efficacy of the drug. Chinese patent CN111808063A discloses a preparation method of olopatadine hydrochloride α-methyl compound, but the corresponding crystal form solubility of the obtained olopatadine hydrochloride α-methyl compound product is relatively poor, and the solid is not easy to disperse. When it takes a long time to stir and disperse, it will further cause difficulty in dispersing durin...

Claims

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Application Information

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IPC IPC(8): C07D313/12A61K31/335A61K9/06A61P17/04A61P17/00
CPCC07D313/12A61K9/06A61P17/04A61P17/00C07B2200/13Y02A50/30
Inventor 张建楼初野常迪赵卫国李佳宝季子建左伟
Owner 唯智医药科技(北京)有限公司
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