Method for preparing crystal form B of pimavanserin semi-tartrate

A technique for hemi-tartrate and pimaserin, which is applied in the field of preparing the hemi-tartrate crystal form B of pimaserine, can solve problems such as difficulties, and achieves the effects of high production efficiency, good economic benefit and simple method

Inactive Publication Date: 2017-07-14
CHENGDU BAIYU PHARMA CO LTD
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  • Abstract
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Problems solved by technology

However, the pimaserin hemitartrate crystal form B still contains some impurities, ...

Method used

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  • Method for preparing crystal form B of pimavanserin semi-tartrate
  • Method for preparing crystal form B of pimavanserin semi-tartrate
  • Method for preparing crystal form B of pimavanserin semi-tartrate

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Embodiment 1

[0037] 1. Pimaserin hemitartrate can be obtained by purchasing commercially available products, or can be prepared by the preparation method of Chinese patent CN102153505 A, and can also be prepared by the following methods:

[0038] 4-isobutoxybenzylamine (17.9g) was dissolved in toluene (73.0g) solution, the toluene solution was cooled to 1-5°C and then hydrogen chloride gas (4.0g) was introduced, keeping the temperature at 10°C, and the , heated to 97-103°C, introduced phosgene (16.2g) through the catheter, after the addition, cooled to 80-85°C, TLC detected that the reaction was complete, stopped the reaction, cooled to room temperature, and obtained a toluene solution of isocyanate.

[0039] At 40°C, the toluene solution of the above isocyanate was added dropwise to a solution of 4-(4-fluorobenzylamino)-1-methylpiperidine (21.7g) in tetrahydrofuran (195g), stirred and reacted for 3 hours, and the reaction was detected by TLC After completion, concentrate under reduced pre...

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Abstract

The invention discloses a method for preparing a crystal form B of pimavanserin semi-tartrate. The method comprises the following steps of adding the pimavanserin semi-tartrate into absolute methanol, stirring, heating, and dissolving; cooling, crystallizing, filtering, and drying, so as to obtain the crystal form B of the pimavanserin semi-tartrate, wherein the weight and volume ratio of the pimavanserin semi-tartrate to the absolute methanol is 1:(4 to 5)g/ml. The method has the advantages that by using the absolute methanol as the solvent, the crystal form B of the pimavanserin semi-tartrate is successfully prepared; the method is simple and convenient, the production efficiency is high, the economic benefit is good, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing pimaserin hemitartrate crystal form B. Background technique [0002] Pimaserin hemitartrate, the chemical name is N-(4-fluorobenzyl)-N-(1-methylpiperidin-4-yl)-N′-(4-(2-methylpropoxy Base) phenylmethyl) urea tartrate (2:1), the English name is urea, N-[(4-fluorophenyl)methyl]-N-(1-methyl-4-piperidinyl)-N′-[[4 -(2-methylpropoxy)phenyl]methyl]-,(2R,3R)-2,3-dihydroxybutanedioate(2:1), is a serotonin 2A receptor inverse agonist, mainly used for the treatment of hallucinations or Parkinson's patients with mental illnesses such as paranoia, its structural formula is as follows: [0003] [0004] Chinese patent CN 102153505 A reports a crystal form B of pipemaserin hemitartrate, which has good stability and water solubility, and its preparation method is as follows: [0005] (1) At 5°C, add 600 μl aqueous solution of 160 mg pipemaserin hemitartrate to 10 ml butanone, stir for 3 days, add 5 ml butanone, and...

Claims

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Application Information

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IPC IPC(8): C07D211/58
CPCC07D211/58C07B2200/13
Inventor 龚胜威甘鹏张振国
Owner CHENGDU BAIYU PHARMA CO LTD
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