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A kind of rupatifene fumarate mixed crystal and preparation method thereof

A fumaric acid, mixed crystal technology, applied in organic chemistry and other directions, to achieve good stability

Active Publication Date: 2017-08-25
FUJIAN MINDONG REJUVENATION PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, no public reports on the crystal form research of rupatifene fumarate have been retrieved. Fujian Mindong Lijiexun Pharmaceutical Co., Ltd. has simultaneously declared the new crystal forms A and B of rupatifene fumarate and their preparation methods. The present invention Provided for the first time the preparation method of the mixed crystal form of rupatifene fumarate crystal form A and B

Method used

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  • A kind of rupatifene fumarate mixed crystal and preparation method thereof
  • A kind of rupatifene fumarate mixed crystal and preparation method thereof
  • A kind of rupatifene fumarate mixed crystal and preparation method thereof

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Embodiment 1

[0020] Dissolve 1.0g rupatifene free base and 1.0g fumaric acid in an appropriate amount of 20ml 95% ethanol solution, stir and react at room temperature for 1hr, concentrate under reduced pressure to 25-30% volume, and cool the solution naturally to room temperature, then in Static crystallization at 2-8°C, rod-shaped crystals precipitated, filtered, washed with 95% ethanol solution at 2-8°C, dried under reduced pressure at 45°C, and obtained.

Embodiment 2

[0022] Weigh 2.0g rupatifene free base and 0.5g fumaric acid and dissolve in an appropriate amount of 50ml 95% ethanol solution, stir and react at room temperature for 2hr, concentrate under reduced pressure to 25-30% volume, and cool the solution naturally to room temperature, then Static crystallization at 2-8°C, rod-shaped crystals precipitated, filtered, washed with 95% ethanol solution at 2-8°C, dried under reduced pressure at 45°C, and obtained.

Embodiment 3

[0024] Dissolve 1.0g rupatifene free base and 2.0g fumaric acid in an appropriate amount of 20ml 95% ethanol solution, stir and react at room temperature for 1hr, concentrate under reduced pressure to 25-30% volume, and cool the solution naturally to room temperature, then Static crystallization at 2-8°C, rod-shaped crystals precipitated, filtered, washed with 95% ethanol solution at 2-8°C, dried under reduced pressure at 45°C, and obtained.

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Abstract

The invention relates to a method for preparing a mixed crystal form of A and B of rupatifen fumarate. The invention relates to a method for preparing a mixed crystal form of 4-[1-(5-methyl-pyridin-3-ylmethyl)-piperidin-4-ylidene]-4,9-dihydro-1-thio-one fumarate shown in the formula (1). The mixed crystal form comprises special characteristic peaks of a crystal form A and a crystal form B; the melting point is 154 + / - 2 DEG C, and the decomposition point is 186 + / - 2 DEG C. The method for preparing the crystal form comprises the following steps of dissolving the free base of rupatifen and fumaric acid in ethanol solution, stirring and reacting for 1 hour at room temperature, concentrating under a reduced pressure to 25-30vol%, or dissolving the rupatifen fumarate crude product in an appropriate amount of ethanol, refluxing in a heating and stirring manner to obtain a saturated solution, naturally cooling the solution prepared in the above method to room temperature, and then standing at 2-8 DEG C to separate out rod-like crystals, filtering, washing with an appropriate amount of ethanol solution of which the temperature is 2-8 DEG C and drying under reduced pressure at 45 DEG C.

Description

technical field [0001] The present invention relates to 4-[1-(5-methyl-pyridin-3-ylmethyl)-piperidin-4-ylidene]-4,9-dihydro-1-thia- A method for preparing mixed crystal forms of benzo[f]azulene-10-one fumarate. Background technique [0002] According to the epidemiological survey results of allergic diseases in 30 countries published by the World Allergy Organization, 22% (250 million people) of the total population of 1.2 billion in these countries suffer from IgE-mediated allergic diseases, such as anaphylaxis. Rhinitis, asthma, conjunctivitis, eczema, food allergy, drug allergy, and severe anaphylaxis affect the quality of life of children and adults, and severe systemic anaphylaxis can even be life-threatening. According to WHO estimates, there are about 150 million asthma patients in the world, of which more than 50% of adults and at least 80% of children are induced by allergic factors, and more than 180,000 people die of asthma every year. [0003] By 2010, 40% to 5...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D409/14
CPCC07D409/14
Inventor 林童俊辛军李琳吴晓华
Owner FUJIAN MINDONG REJUVENATION PHARMA
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