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Brexpiprazole purifying method

A technology of epirazole and a refining method, applied to the refining field of epirazole, can solve the problems of insignificant refining effect, cumbersome operation steps, low refining yield, etc., and achieves high product yield, good refining effect, Simple to use effects

Inactive Publication Date: 2016-12-07
山东川成医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the prior art, using ethanol as a solvent, adding an appropriate amount of concentrated hydrochloric acid to prepare hydrochloride, recrystallization, and then adjusting the base with sodium hydroxide solution to obtain the desired product, this method has cumbersome steps and a low refining yield. And the purity is not high, the refining effect is not obvious, and it needs to be refined twice or even multiple times, so although the purity is improved, the yield is greatly reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation of the crude product of epizopine refers to the preparation of the patent CN104254530

[0028] (1) Synthesis of 7-(4-chlorobutoxy)-1H-quinolin-2-one

[0029] Methanol (14.9 L), 7-hydroxy-1H-quinolin-2-one (1.487 kg) and potassium hydroxide (0.621 kg) were mixed and stirred. After dissolution, 1-bromo-4-chlorobutane (4.746 kg) was further added thereto, and the resulting mixture was stirred under reflux for 7 hours. Then, the mixture was stirred at 10°C for one hour. The precipitated crystals were centrifuged and washed with methanol (1.5 L). Wet crystals are collected and jarred. Water (14.9 L) was added thereto, followed by stirring at room temperature. After centrifugation, the resulting solid was washed with water (3 L). Wet crystals are collected and packed into jars. After methanol (7.4 L) was added, the mixture was stirred at reflux for one hour, cooled to 10° C., and then stirred. The precipitated crystals were centrifuged and washed with m...

Embodiment 2

[0032] The refining of embodiment 2 epizopine crude product

[0033] Mix 100g of crude epizopyr with 800ml of acetone, raise the temperature to reflux, stir for about 15 minutes to dissolve the solid, then add 20g of activated carbon, decolorize for 30 minutes, heat filter, the filtrate naturally cools to room temperature, heat preservation and crystallization for 2 hours, filter, cool Wash with 100 milliliters of acetone to obtain 90.0 g of refined product with a yield of 90.0% and a purity of 99.5%.

Embodiment 3

[0034] The refining of embodiment 3 epizole crude product

[0035] Mix 100g of crude Ipizopine with 600ml of acetone, raise the temperature to reflux, stir for about 15 minutes to dissolve the solid, then add 20g of activated carbon, decolorize for 30 minutes, heat filter, the filtrate naturally cools to room temperature, heat preservation and crystallization for 2 hours, filter, cool Wash with 100 milliliters of acetone to obtain 86.9 g of refined product with a yield of 86.9% and a purity of 99.2%.

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Abstract

The invention belongs to the technical field of chemical synthesis, and concretely relates to a brexpiprazole purifying method. The method comprises the following steps: mixing crude brexpiprazole with acetone, heating the obtained mixture until the mixture is refluxed, stirring until solid is dissolved, adding active carbon to decolorize, carrying out hot filtration, naturally cooling the obtained filtrate to room temperature, carrying out heat insulation crystallization, and washing the obtained filtered solid with cold acetone to obtain purified brexpiprazole. The brexpiprazole purifying method has the advantages of good purifying effect, high product yield, low cost, and simplicity in operation, and is especially suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for refining epirazole. Background technique [0002] The English name of Epirazole is brexpiprazole, its alias is OPC-34712, its chemical name is 7-(4-(4-(benzo[b]thiophen-4-yl-piperazin-1-yl)butoxy)-1H- Quinolin-2-one, CAS is 913611-97-9 Molecular formula is C 25 h 27 N 3 o 2 S phase, the relative molecular mass is 433.57, the original research company is Otsuka Pharmaceutical Co., Ltd., and the indications are schizophrenia and depression. Currently, FDA has approved it for marketing. The structural formula of epizopine is: [0003] . [0004] There are relatively few reports on the synthesis method of Epirizole at present. Patent CN104254530 discloses a preparation method of Epirizole, specifically: (1) 7-(4-Chlorobutoxy)-1H-quinoline-2- Ketone synthesis [0005] Methanol (149 L), 7-hydroxy-1H-quinolin-2-one (14.87 kg) and potassium h...

Claims

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Application Information

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IPC IPC(8): C07D409/12
CPCC07D409/12
Inventor 马居良郭明刘怀振
Owner 山东川成医药有限公司
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