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New preparation method of Blonanserin intermediate

A technology for blonanserin and intermediates, which is applied in the field of preparation of blonanserin intermediates, can solve problems such as complicated operations, and achieve the effects of simple reaction steps, high yield and simple post-processing

Active Publication Date: 2012-12-19
常州华生制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN 101747273A discloses the synthesis method of formula I, the reaction will be carried out in two steps, and a large amount of polyphosphoric acid will be used, the operation is complicated

Method used

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  • New preparation method of Blonanserin intermediate
  • New preparation method of Blonanserin intermediate
  • New preparation method of Blonanserin intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put 100ml of toluene, 5g of p-fluorobenzoylacetonitrile (II), 5g of cyclooctanone (III), 5g of p-toluenesulfonic acid, and 5ml of concentrated sulfuric acid into the reaction bottle, heat and stir at about 110°C for 3 hours, and after the central control reaction is complete , adding water to wash, extract and separate layers, and the organic layer was decolorized and concentrated to obtain 6.8 g of crystals. The yield is 82%, the purity is 98.4%, and the melting point is 236-238°C.

Embodiment 2

[0022] Put 150ml of toluene, 10g of p-toluenesulfonic acid into the reaction bottle, heat and stir, continue to add 5g of p-fluorobenzoylacetonitrile, 5g of cyclooctanone and 5ml of concentrated sulfuric acid, and reflux at about 110°C for 3 hours. After the central control reaction is complete, add water After washing, extracting and separating the layers, the organic layer was decolorized and concentrated to obtain 7 g of crystals. The yield is 85%, the purity is 98.5%, and the melting point is 236-238°C.

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PUM

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Abstract

The invention discloses a preparation method of a Blonanserin intermediate. In the method, 4-fluorobenzoylacetonitrile reacts with cyclooctanone to generate 4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydrocycloocta pyridine-2(1H)-ketone at a high yield in the presence of a catalyst.

Description

technical field [0001] The present invention relates to blonanserin intermediate 4-(4-fluorophenyl)-5,6,7,8,9,10,-hexahydrocyclooctanopyridin-2(1H)-one (I) Prepare a new method. Background technique [0002] The blonanserin intermediate described in this specification refers to 4-(4-fluorophenyl)-5,6,7,8,9,10,-hexahydrocyclooctanopyridin-2(1H)-one ( 1), this compound is the key intermediate in the synthetic process of the antipsychotic drug Blonanserin (Blonanserin) of a new generation. [0003] JP4099768A and EP0385237 have reported the synthetic method of formula I compound, and this method uses 4-fluorobenzoylacetonitrile (II) and cyclooctanone (III) to react at 120 ℃ in the presence of polyphosphoric acid, and the yield reported in the literature is 60 %, but the inventor prepared 4-(4-fluorophenyl)-5,6,7,8,9,10,-hexahydrocyclooctanopyridin-2(1H)-one (I ), the yield is only about 18%. And will use a large amount of polyphosphoric acid, produce a large amount of waste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/04
Inventor 钟海涛奚小金
Owner 常州华生制药有限公司
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