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Method for preparing high-purity blonanserin

A blonanserin and high-purity technology, applied in organic chemistry and other fields, can solve problems such as long reaction routes, high costs, and gaps

Inactive Publication Date: 2016-02-10
高瑞耀业(北京)科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] For Route 1: The reaction route is relatively long, and the yield of the ring-closing reaction of 3-(4-fluorophenyl)-3-oxopropanamide and cyclooctanone is very low, and it is difficult to control the cost in industrial production
[0011] For Route 2: This route has fewer reaction steps, but the yield reported in the literature is very low and the cost is high, which needs to be further optimized
Moreover, the research work that has been reported at present is all small-scale explorations carried out under laboratory conditions, and there is still a large gap with industrialized production.

Method used

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  • Method for preparing high-purity blonanserin
  • Method for preparing high-purity blonanserin
  • Method for preparing high-purity blonanserin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 15kg polyphosphoric acid and 6750g phosphoric acid into the reactor, start stirring, the system is heated up to 55-60°C, add 1500g p-fluorobenzoylacetonitrile in batches, continue stirring for 10min, add 667g cyclooctanone in batches, and keep warm for 30min , heating to raise the temperature of the system to 105-110°C, follow the reaction, after 2.5h, add 167.5g cyclooctanone, continue the reaction for about 1.5h, add 167.5g cyclooctanone again, follow the reaction until the reaction of the raw materials is complete , cool the reaction system and keep the temperature between 80 and 90°C, slowly add 13.5 LDMF dropwise, after the drop is complete, pour the reaction solution into 300L water, stir, after 30min, add 1L of petroleum ether, a yellow solid precipitates, continue to stir for 1h , filtered, the filter cake was washed with petroleum ether, and dried to obtain 900.5g of solid, which was refined by adding 1L of isopropanol to obtain 868.6g of yellow solid, with ...

Embodiment 2

[0032] Add 15kg polyphosphoric acid and 6750g phosphoric acid into the reactor, start stirring, the system is heated up to 55-60°C, add 1500g p-fluorobenzoylacetonitrile in batches, continue stirring for 10min, add 667g cyclooctanone in batches, and keep warm for 30min , heating to raise the temperature of the system to 115-120°C, follow the reaction, after 2.5h, add 167.5g cyclooctanone, continue the reaction for about 1.5h, add 167.5g cyclooctanone again, follow the reaction until the reaction of the raw materials is complete , cool the reaction system and keep the temperature between 80 and 90°C, slowly add 13.5 LDMF dropwise, after the drop is complete, pour the reaction solution into 300L water, stir, after 30min, add 1L of petroleum ether, a yellow solid precipitates, continue to stir for 1h , filtered, the filter cake was washed with petroleum ether, and dried to obtain 853.8g of solid, which was refined by adding 1L of isopropanol to obtain 821.3g of yellow solid, with ...

Embodiment 3

[0034] Add 15kg polyphosphoric acid and 6750g phosphoric acid into the reactor, start stirring, the system is heated up to 55-60°C, add 1500g p-fluorobenzoylacetonitrile in batches, continue stirring for 10min, add 667g cyclooctanone in batches, and keep warm for 30min. Heating to raise the temperature of the system to 105-110°C, follow the reaction, after 2.5 hours, add 167.5g cyclooctanone, continue the reaction for about 1.5h, add 167.5g cyclooctanone again, follow the reaction until the reaction of the raw materials is complete, Cool the reaction system and keep the temperature between 80 and 90°C, slowly add 13.5L of ethyl acetate dropwise, after the drop is complete, pour the reaction solution into 300L of water, stir, after 30min, add 1L of petroleum ether, a yellow solid precipitates, continue Stir for 1 h, filter, wash the filter cake with petroleum ether, and dry to obtain 832.4 g of solid, add 1 L of isopropanol to refine, obtain 802.1 g of yellow solid, which is the...

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Abstract

The invention relates to a new preparation method for blonanserin shown as a formula (I) in the specification. The provided new method for preparing high-purity blonanserin shown as the formula (I) is economic and effective. The crude product of the formula (I) compound obtained through the method possesses the purity of 99.5%, and blonanserin with the single-impurity content less than 0.1% is obtained after being refined.

Description

field of invention [0001] The invention relates to an economical and effective method for preparing high-purity blonanserin. The crude product of blonanserin obtained by the method of the invention has a purity of up to 99.5%. Southern Forest. Background of the invention [0002] Blonanserin, chemical name 2-(4-ethyl-1-piperazinyl)-4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydro Cycloocta[b]pyridine, developed by Sumitomo Pharmaceutical Co., Ltd., was first launched in Japan in April 2008. This product is a highly selective 5-HT2 receptor and D2 receptor antagonist, with low affinity for D1 and adrenal hormone α1, H1 histamine receptor and M1 choline receptor, and is mainly used in the treatment of atypical psychosis clinically . [0003] For the synthesis of blonanserin, the reported process route is as follows: [0004] 1. Route 1: Using methyl p-fluorobenzoate as the starting material, first react with acetonitrile to prepare p-fluorobenzoylacetonitrile, and react in polyph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/04
Inventor 高雪松沈刚赵鹏杜红丽刘明
Owner 高瑞耀业(北京)科技有限公司
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