New crystal form XVII of 1-(4-(5-cyanoindole-3-yl) butyl)-4-(2-carbamyl-benzofuran-5-yl)-piperazine hydrochloride and preparation method of new crystal form XVII

A cyanoindole, benzofuran technology, applied in the field of organic chemistry, can solve the problems of large difference in solubility of dehydrate crystal forms, poor crystal form stability and the like

Inactive Publication Date: 2013-03-20
NANJING HEALTHNICE MEDICAL TECH
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AI Technical Summary

Problems solved by technology

[0004] 1-[4-(5-cyanindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine hydrochloride has now found 16 different Pure crystals and their preparation methods, of which 6 solvate crystal forms cannot be used for medicine, 3 hydrate crystal forms have poor stability, 4 dehydrate crystal forms have large solubility differences, and the rest are 1-[ 4-(5-cyanindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine dihydrochloride is not used in medicine, and the above crystal forms are all different from the present invention

Method used

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  • New crystal form XVII of 1-(4-(5-cyanoindole-3-yl) butyl)-4-(2-carbamyl-benzofuran-5-yl)-piperazine hydrochloride and preparation method of new crystal form XVII
  • New crystal form XVII of 1-(4-(5-cyanoindole-3-yl) butyl)-4-(2-carbamyl-benzofuran-5-yl)-piperazine hydrochloride and preparation method of new crystal form XVII
  • New crystal form XVII of 1-(4-(5-cyanoindole-3-yl) butyl)-4-(2-carbamyl-benzofuran-5-yl)-piperazine hydrochloride and preparation method of new crystal form XVII

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Embodiment 1

[0017] Example 1, New crystal of 1-[4-(5-cyanindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine hydrochloride Preparation of Form XVII

[0018] Add 21 g Hydrochloric acid (37%). After stirring, the precipitated crystals were suction-filtered and dried in vacuum at 85 to 90°C to constant weight to obtain 1-[4-(5-cyanindol-3-yl)butyl]-4-(2 -carbamoyl-benzofuran-5-yl)-piperazine hydrochloride. The obtained 1-[4-(5-cyanindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine hydrochloride and water according to Mixed at a ratio of 1:5 to 1:10, after stirring, the precipitated crystals were suction filtered, dried in vacuum at 80 to 90°C to constant weight, and dried to obtain 1-[4-(5-cyanindole-3 -yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine hydrochloride new crystal form X VII.

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Abstract

The invention relates to a new crystal form XVII of 1-(4-(5-cyanoindole-3-yl) butyl)-4-(2-carbamyl-benzofuran-5-yl)-piperazine hydrochloride and a preparation method of the new crystal form XVII. Peaks of an X-ray diffraction pattern of powder of the new crystal form XVII are located at 9.02 degrees, 9.96 degrees, 13.06 degrees, 20.90 degrees, 21.32 degrees, 22.94 degrees, 23.70 degrees and 24.62 degrees+ / -0.2 degrees and 2 theta, initial melting is shown at about 277 DEG C in a differential scanning calorimetry spectrum, and thermogravimetric analysis shows that the product has no water of crystallization.

Description

field of invention [0001] The present invention relates to the field of organic chemistry and pharmacy, in particular to formula (I) 1-[4-(5-cyanindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran- New crystalline form XVII of 5-yl)-piperazine hydrochloride and process for its preparation. [0002] Background technique [0003] Certain crystalline, i.e., morphological forms of a pharmaceutical compound may aid in the development of a suitable dosage form, as the exact dose used or measured may differ between batches if the morphological form is not kept constant during clinical and stability studies. There is no comparison between them. Once a useful compound has been prepared, it is important to recognize the morphological form that is present in each dosage form to ensure that the manufacturing process uses the same form and includes the same amount of drug in each dose. [0004] 1-[4-(5-cyanindol-3-yl)butyl]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine hydrochloride has now fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/12
Inventor 邹巧根葛敏兰公剑周惠宏
Owner NANJING HEALTHNICE MEDICAL TECH
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