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High-purity blonanserin and preparation method thereof

A technology of piperazinyl and compound, which is applied in the field of high-purity blonanserin and its preparation, and achieves the effects of low cost, favorable industrial production, and easy and controllable reaction

Active Publication Date: 2013-09-18
AVENTIS PHARMA HAINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

I

Method used

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  • High-purity blonanserin and preparation method thereof
  • High-purity blonanserin and preparation method thereof
  • High-purity blonanserin and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0026] Add 163g of compound III, 380g of cyclooctanone, 5g of cyclohexylamine and RuH to a 2L three-neck flask 2 (PPh 3 ) 0.5g, heated to 160-170°C. The reaction was stirred for 5 hours, and the reaction was detected by TLC. After the reaction was completed, the temperature was lowered to 70° C., 100 ml of isopropanol was added, stirred while naturally cooling to room temperature, suction filtered, and the filter cake was dried to constant weight to obtain 211 g of the compound of formula II with a yield of 76%. Melting point: 236-239°C, HPLC purity 98%.

Embodiment 2

[0028] Remove 200 g of compound II obtained above, add 300 ml of phosphorus oxychloride, and heat to reflux for 2 hours. After cooling to room temperature, 2 L of chloroform was added to the mixture, and washed with saturated sodium carbonate. The organic phase was separated, dried with anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified with isopropanol to obtain 154 g of a solid product with a yield of 71%. Melting point: 111-112°C, HPLC purity 98%.

Embodiment 3

[0030] 140 g of Compound III obtained above, 150 g of methylpiperazine, 50 g of sodium iodide and 2 L of toluene were mixed and refluxed for 12 hours, cooled to room temperature, and washed with saturated sodium carbonate. The organic phase was separated, dried with anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified with isopropanol to obtain 123 g of a solid product with a yield of 78%. Melting point: 133-135°C, HPLC purity 99.5%.

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Abstract

The invention discloses a high-purity 2-(4-ethyl-1-piperazinyl)-4-(4-fluorophenyl)-5, 6, 7, 8, 9, 10-hexahydro-cycloocta-(b) pyridine and a preparation method thereof. The target product of the invention can be applied to the treatment of schizophrenia, with higher safety and effectiveness. The preparation method has mild reaction condition and simple post treatment, and can obtain high-purity final products and is easier to implement industrialized production.

Description

technical field [0001] The present invention relates to a high-purity stable 2-(4-ethyl-1-piperazinyl)-4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydroaromatic The octa[b]pyridine and its preparation method can be used as medicine for treating schizophrenia. Background technique [0002] Blonanserin, chemical name: 2-(4-ethyl-1-piperazinyl)-4-(4-fluorophenyl)-5,6,7,8,9,10-hexa Hydroaromatic octa[b]pyridines. It is a drug for treating mental and nervous diseases, and can be used for the treatment of schizophrenia. Its chemical structural formula is as follows: [0003] [0004] A common method for preparing a compound of formula I is disclosed in EP0385237, and its reaction scheme is as follows: [0005] [0006] In the first step reaction of the above route, polyphosphoric acid is used as a catalyst to generate a ring-closing reaction, wherein the amount of polyphosphoric acid is 10 times that of the reactant. The disposal of the three wastes brings trouble. Not suitable...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/04A61P25/18
Inventor 张海平
Owner AVENTIS PHARMA HAINAN
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