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Crisaborole crystal form compound and preparation method thereof

A technology for crisaborol and compounds, which is applied in the field of crisaborol crystal compounds and their preparation, can solve the problems of difficult control of crystal particle size and crystal form changes, etc., and achieve suitable for large-scale industrial production, good stability, The effect of mild preparation conditions

Inactive Publication Date: 2021-02-19
JIANGSU SEMPOLL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size of the crystals prepared according to the reported method is not easy to control, and there is a phenomenon of crystal form changes after a period of time, which poses challenges to the development of preparations

Method used

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  • Crisaborole crystal form compound and preparation method thereof
  • Crisaborole crystal form compound and preparation method thereof
  • Crisaborole crystal form compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0038] Embodiment: Preparation of crisborole crystal compound

[0039] According to the method reported in patent CN10347965, 100 g of crude crisborole was prepared.

[0040] Take 20g of Criborol into a reaction bottle, add 40ml of analytically pure ethyl acetate solvent, heat to 76-82°C, stir to dissolve, then filter while hot, after filtration, the reaction heat is cooled to 20-30°C while stirring (cooling The range is 1-2°C every 10 minutes), after 2 hours of heat preservation, continue to cool down to 0-10°C, and keep the crystal for 1-3 hours. Vacuum filtration, and the filter cake was dried in a blast oven at 60°C for 8 hours to obtain 16.3 g of white crystalline solid powder.

[0041] Further illustrate the present invention by experimental example below:

experiment example 1

[0042] Experimental Example 1: Solubility Determination

[0043] Refer to the Chinese Pharmacopoeia 2015 version to determine its solubility. Method: take an appropriate amount of this product, add ethanol respectively, shake vigorously for 30 seconds every 5 minutes, and observe the dissolution within 30 minutes. The results are shown in Table 1.

[0044] Table 1 Crystal form solubility test result of the present invention

[0045]

experiment example 2

[0046] Experimental Example 2: Stability Test

[0047] In this experimental example, the stability of the crisborole crystals provided by the present invention is investigated through accelerated tests and long-term tests.

[0048] Take the samples prepared in the examples, and place them for 6 months under the conditions of temperature 40±2°C, relative humidity 75±5% and temperature 25±5°C, relative humidity 60±5%, and take samples at the end of 0, 3, and 6 months respectively Determination of properties, related substances and content, the results are shown in Table 2.

[0049] Table 2: Accelerated and long-term stability test results

[0050]

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Abstract

The invention belongs to the technical field of medicine, and discloses a crisaborole crystal form compound and a preparation method thereof. The crisaborole crystal form compound displays characteristic diffraction peaks at 2[theta]+ / -0.2 degree of 6.02 degrees, 12.04 degrees, 15.13 degrees, 15.35 degrees, 18.09 degrees, 24.20 degrees and 26.08 degrees in an X-ray powder diffraction pattern, andthe X-ray powder diffraction pattern obtained through Cu-K alpha ray measurement is completely different from the prior art. According to the invention, the crisaborole crystal form compound has goodwater solubility and high stability, the preparation method is simple and easy to operate, the medication safety is greatly improved after the compound is prepared into a pharmaceutical composition, and the crisaborole crystal form compound is very suitable for clinical application.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a crisborole crystal compound and a preparation method thereof. Background technique [0002] Crisaborole (trade name Eucrisa, Crisaborole ointment) is a boron-based topical phosphodiesterase-4 (PDE-4) inhibitor, which was purchased by Pfizer from Anacor for $5.2 billion. The drug was approved by the US FDA in 2016 for the treatment of mild to moderate atopic dermatitis (AD) in children and adults aged 2 and over. It is the first new small molecule drug approved by the FDA for the treatment of AD in 15 years. [0003] The chemical name of crisborole is: 5-(4-cyanophenoxy)-1,3-dihydro-1-hydroxy-[2,1]-benzoxaborole, and its chemical structure is shown in formula (I): [0004] [0005] (I) [0006] PCT application WO2017193914 discloses the crystalline form of crisborole in its free form, its preparation method and use, and it reports four crystalline forms of crisborole I, II, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/025C07B2200/13
Inventor 鲍丰祺蔡蓓蕾顾敏龚培颖王金玲
Owner JIANGSU SEMPOLL PHARMA
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