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Purification method of asenapine

A purification method and drying technology, applied in the field of medicine, can solve the problems of unfavorable industrial production, cumbersome reaction process, low yield and the like, and achieve the effects of small solvent consumption, controllable purification conditions and simple operation.

Inactive Publication Date: 2018-03-06
TIANJIN HANKANG PHARMA BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present inventor still has complex and loaded down with trivial details reaction process through the research of above-mentioned method, is unfavorable for suitability for industrialized production, and purity is low, problems such as low yield, be badly in need of developing a kind of new asenapine purification method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 30 grams of crude asenapine was dissolved in 60 ml of methanol, cooled to 0°C, and left to crystallize at 0°C for 10 hours. After suction filtration, the filter cake was collected and vacuum-dried to obtain 27.4 grams of crude product;

[0020] Dissolve 27.4 g of the dried crude product in a mixed solution of 252 g of acetonitrile-water ~ 3:1, stir and dissolve, then stand for crystallization at 0°C for 48 hours, collect the filter cake after suction filtration, and place the filter cake in a vacuum-dried Drying under reduced pressure in the oven, the vacuum degree was controlled at -0.085MPa, and the temperature was controlled at 10°C for 32 hours to obtain 26.4 g of the target product asenapine, with a purity of 99.95% as detected by HPLC.

Embodiment 2

[0022] Dissolve 30 grams of crude asenapine in 100 ml of isopropanol, cool to 8°C, and stand at 10°C for crystallization for 12 hours. After suction filtration, the filter cake is collected and vacuum-dried to obtain 27.9 grams of crude product;

[0023] Dissolve 27.9 grams of the dried crude product in 390 ml of acetonitrile-water=3:1 mixed solution, stir evenly, and then stand for crystallization at 8°C for 24 hours, collect the filter cake after suction filtration, and place the filter cake in a vacuum-dried Drying under reduced pressure in the box, the vacuum degree is controlled above -0.09MPa, and the temperature is controlled at 25°C for 15 hours to obtain 26 grams of the target product asenapine, the purity of which is 99.92% by HPLC.

Embodiment 3

[0025] Dissolve 30 grams of crude asenapine in 100 ml of isobutanol, cool to 10°C, and stand at 15°C for crystallization for 15 hours. After suction filtration, the filter cake is collected and vacuum-dried to obtain 26.8 grams of crude product;

[0026] 26.8 grams of the dried crude product were dissolved in 130 ml of tetrahydrofuran-water mixed solution with a volume ratio of 3:1, stirred and dissolved, and left to crystallize at 10° C. for 12 hours. After suction filtration, the filter cake was collected, and the filter cake was placed in Drying under reduced pressure in a vacuum drying oven with the vacuum degree controlled at -0.09MPa and the temperature controlled at 45°C for 32 hours yielded 26.4 g of the target product asenapine, with a purity of 99.93% as detected by HPLC.

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PUM

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Abstract

The invention discloses a method for purifying asenapine. The method carries out crystallization and purification through two different crystallization systems, and adopts a low-temperature drying method to purify asenapine. The purity of asenapine in the purified product reaches 99.9% % above, the total impurity content does not exceed 0.1%, and does not contain adsorbed water.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a method for purifying asenapine. Background technique [0002] Asenapine, the chemical name is trans-5-chloro-2,3,3a,12b-tetrahydro-2-methyl-1H-dibenzo[2,3:6,7]oxa Zhuo[4,5-c]pyrrole has CNS-inhibitor activity, antihistamine and anti-serotonin activity, and its maleate is clinically used. Asenapine maleate (also known as asenapine maleate) can be made into pharmaceutical preparations for sublingual or oral administration (see international application patent WO / 23600), which is clinically applicable to adults with schizophrenia, Emergency treatment of psychiatric disorders such as mania or mixed episodes with type 1 bipolar disorder, the trade name is Saphris. The extensive clinical research and application of asenapine maleate necessitates the large-scale synthesis of the drug. [0003] A large amount of research has been carried out to the synthesis of asenapine both at home and abr...

Claims

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Application Information

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IPC IPC(8): C07D491/044
CPCC07D491/044
Inventor 严洁
Owner TIANJIN HANKANG PHARMA BIOTECH
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