Method for preparing pimavanserin hemitartrate crystal form B

A technology of hemitartrate and pipemaserin, which is applied in the field of preparation of pipemaserin hemitartrate crystal form B, can solve the problems of poor economic benefit, low production efficiency, unsuitable for industrial production, etc., and achieve good economic benefit , high production efficiency and simple method

Active Publication Date: 2016-08-17
CHENGDU BAIYU PHARMA CO LTD
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Problems solved by technology

[0008] The preparation method of the above-mentioned crystal form B not only needs to use organic solvents such as butanone and toluene which are toxic and harmful to the human body, which seriously affects the safety of the use of pipemaserin hemitartrate crystal form B as a drug, and the method is used in organic solvents. The mixing time is as long as 18 hours to 3 days, the production efficiency is very low, the economic benefit is poor, and it is not suitable for industrial production

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  • Method for preparing pimavanserin hemitartrate crystal form B
  • Method for preparing pimavanserin hemitartrate crystal form B
  • Method for preparing pimavanserin hemitartrate crystal form B

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Embodiment 1

[0036] 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:

[0037] 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.

[0038] 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 pimavanserin hemitartrate crystal form B. The method comprises the following steps: adding pimavanserin hemitartrate into water; and after the pimavanserin hemitartrate is dissolved, concentrating and drying to obtain the pimavanserin hemitartrate crystal form B, wherein the weight-to-volume ratio of the pimavanserin hemitartrate to the water is 1:(4-6) g / ml. By using the nontoxic harmless water as the solvent, the pimavanserin hemitartrate crystal form B is successfully prepared. Besides, the method is simple and convenient, has the advantages of high safety, environment friendliness, high production efficiency and favorable economic benefits, and is very 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/58
CPCC07B2200/13C07D211/58
Inventor 龚胜威甘鹏张振国
Owner CHENGDU BAIYU PHARMA CO LTD
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