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New preparation method of Blonanserin intermediate

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

Active Publication Date: 2011-06-15
常州华生制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And a large amount of polyphosphoric acid is used, a large amount of waste water is generated, and the operation is complicated
[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 flask. Heat and stir at about 110°C and reflux for 3 hours. After the central control reaction is complete After adding water to wash, extract and separate the layers, the organic layer is decolorized and concentrated to obtain 6.8g 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 flask, heat and stir, continue to add 5g of p-fluorobenzoylacetonitrile, 5g of cyclooctanone and 5ml of concentrated sulfuric acid, reflux for 3 hours at about 110℃, add water after the control reaction is complete Washing, extracting and separating, the organic layer is 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 the intermediate 4-(4-fluorophenyl)-5,6,7,8,9,10,-hexahydrocyclooctanopyridine-2(1H)-one (I) of branserin Preparation of new methods. Background technique [0002] The blonanserin intermediate mentioned in this specification refers to 4-(4-fluorophenyl)-5,6,7,8,9,10,-hexahydrocyclooctanopyridine-2(1H)-one ( I), the compound is a key intermediate in the synthesis of a new generation of anti-schizophrenic drug Blonaserin (Blonanserin). [0003] JP4099768A and EP0385237 report the synthesis method of the compound of formula I. The method uses 4-fluorobenzoylacetonitrile (II) and cyclooctanone (III) to react at 120°C in the presence of polyphosphoric acid. The literature reported a yield of 60 %, but the inventors prepared 4-(4-fluorophenyl)-5,6,7,8,9,10,-hexahydrocyclooctanopyridine-2(1H)-one (I ), the yield is only about 18%. In addition, a large amount of polyphosphoric acid is used, a large amount of waste water is generat...

Claims

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Application Information

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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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