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Crystal form and preparation method of clomipamine hydrochloride

A technology of clomipramine hydrochloride and crystal form, which is applied in the field of drug crystal form, can solve the problems of no clomipramine hydrochloride, etc., and achieve the effect of stable crystal form

Active Publication Date: 2021-03-09
HUNAN DONGTING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The melting point of clomipramine hydrochloride crystals is 191.6-194.8°C. At present, there is no report on the crystal forms of clomipramine hydrochloride or such drugs in China

Method used

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  • Crystal form and preparation method of clomipamine hydrochloride
  • Crystal form and preparation method of clomipamine hydrochloride
  • Crystal form and preparation method of clomipamine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Preparation route of the present invention:

[0029] Using the commercially available sangite of formula I as the starting material, the hydrolyzate of formula II is obtained by hydrolysis under alkaline conditions (refer to existing patents). The difference in this process is that the commercially available side chain (N, N-dimethyl chloropropane hydrochloride) to prepare the formula III condensate, the formula III condensate is formed into a salt by feeding HCl gas into the toluene solution to prepare clomipramine hydrochloride.

[0030] (1) Preparation of hydrolyzate

[0031]

[0032] (2) Preparation of condensate

[0033]

[0034] (3) Preparation of crude product

[0035]

[0036] (4) Preparation of high-quality goods

[0037]

[0038] Step (1) and step (2) of the present invention are the same as the prior art (for example, the patent application number is CN202010632533.7), step (3) is, 50g clomipramine is added in 250g toluene, then pass through I...

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Abstract

The invention belongs to the technical field of medicine crystal forms, and particularly relates to a clomipamine hydrochloride crystal form and a preparation method, and the melting point of clomipamine hydrochloride is 185.1-188.6 DEG C, in an X-ray diffraction pattern scanned by CuK alpha radiation and 2theta (degrees, + / -0.2), diffraction peaks exist at 5.70 degrees, 17.17 degrees, 19.77 degrees and 22.98 degrees, the relative abundance exceeds 50%, diffraction peaks exist at the positions of 20.21 degrees and 28.83 degrees, the relative abundance is 30%-50%, the clomipamine hydrochloridehas diffraction peaks at 23.67 degrees, 24.68 degrees and 29.99 degrees, the relative abundance is 10%-20%, the purity of the clomipamine hydrochloride is high and reaches 99.9%, the single maximum impurity content is 0.02%, and the stability is good.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical crystal forms, and in particular relates to a crystal form of clomipramine hydrochloride and a preparation method. Background technique [0002] Clomipramine Hydrochloride (Clomipramine Hydrochloride), chemical name: N,N-dimethyl-10,11-dihydro-3-chloro-5H-dibenzo(b,f)azepine Hydrochloride, its structural formula is as follows: [0003] [0004] Physical and chemical properties: This product is white or slightly yellow crystalline powder, odorless, bitter in taste, and gradually turns yellow when exposed to light. This product is acidic, with a pH value between 3.5 and 5.0. This product is very soluble in glacial acetic acid, easily soluble in water, methanol, chloroform, soluble in ethanol, slightly soluble in anhydrous acetic acid, slightly soluble in acetone, almost insoluble in ethyl acetate and ether. [0005] Clomipramine hydrochloride is a tricyclic antidepressant. It is clinic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/28
CPCC07D223/28C07B2200/13
Inventor 柳静侯奇伟张莉丽王波符万里赵国权刘源
Owner HUNAN DONGTING PHARMA
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