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Clozapine impurity as well as preparation method and application thereof

A clozapine and impurity technology, applied in the field of pharmaceutical preparations, can solve the problems of difficult operation and treatment, reduce the effect, increase the burden on patients, etc., and achieve the effects of simple post-processing, simple operation and high yield

Inactive Publication Date: 2018-06-08
艾希尔(深圳)药物研发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Considering the impact of impurities in the drug, the less the content of impurities, the better, but if the impurities are to be completely removed, it will inevitably cause difficulties in production operations, increase production costs, reduce efficacy, and increase the burden on patients economically.
On the other hand, to remove impurities is not necessary for the efficacy, storage, and adjustment of drugs, and it is not possible to completely remove impurities.

Method used

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  • Clozapine impurity as well as preparation method and application thereof
  • Clozapine impurity as well as preparation method and application thereof
  • Clozapine impurity as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment

[0028] The preparation of embodiment clozapine impurity

[0029] Add 4-chloro-2-nitroaniline (1.0 g, 5.79 mmol, 1.0 eq), o-iodobenzoic acid (1.72 g, 6.95 mmol, 1.20 eq), K 2 CO 3 (1.6 g, 11.59 mmol, 2.0 eq), CuI (0.111 g, 0.58 mmol, and DMF20 mL), vacuumize, replace with argon three times, and finally stir and heat up to 120 °C under the protection of argon, react for 2 hours, and the reaction is complete , add water and stir, extract with n-butanol, concentrate the organic layer, and recrystallize from isopropanol to obtain 1.50 g of SM1 brown solid, with a yield of 88%.

[0030] Add SM1 (1.0 g, 3.42 mmol, 1.0 eq), oxalyl chloride (0.867 g, 6.83 mmol, 2.0 eq) and anhydrous dichloromethane (20 ml) into a 100 mL round bottom flask successively, stir at room temperature for 30 min, spin to dry the solvent, Excess oxalyl chloride was removed, and anhydrous dichloromethane (20ml) was added to the solid under ice bath, followed by triethylamine (1.38g, 13.67mmol, 4eq) and N-methy...

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Abstract

The invention discloses a clozapine impurity and a preparation method thereof. The preparation method comprises the following steps: carrying out a reaction by taking o-iodobenzoic acid and 4-chloro-2-nitroaniline as starting reactants and using one or more of halogen copper salts, carbonates and phosphates as catalysts so as to generate an intermediate SM1; mixing the intermediate SM1, oxalyl chloride and N-methyl piperazine, and using a one-pot method to synthesize an intermediate SM2; reducing the intermediate SM2 in an acid environment by using metal powder so as to obtain the clozapine impurity. The invention discloses a clozapine impurity compound and a preparation method thereof for the first time, and the technology of the preparation method of the impurity appears for the first time; furthermore, the method is simple to operate and easy in aftertreatment; the prepared clozapine impurity is high in purity and yield.

Description

technical field [0001] The invention belongs to the field of pharmaceutical preparations, specifically relates to a clozapine impurity, and provides a preparation method of the clozapine impurity and its application as an impurity reference substance. Background technique [0002] Impurities in drugs refer to substances that have no therapeutic effect, affect the stability and efficacy of drugs, or are even harmful to human health. The existence of these substances not only affects the quality of the drug, but also reflects the problems in the production and storage process. The inspection of impurities contained in medicines can not only ensure the safety and effectiveness of medicines, but also provide a basis for the quality assurance of production and distribution processes and the assessment of enterprise management. Impurities in drugs can be divided into general impurities and special impurities according to their sources. General impurities refer to impurities that...

Claims

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Application Information

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IPC IPC(8): C07C237/30C07C231/02C07C231/12C07C227/08C07C229/58G01N1/28
CPCC07C227/08C07C231/02C07C231/12C07C237/30G01N1/28C07C229/58
Inventor 周佳李方林肖海新
Owner 艾希尔(深圳)药物研发有限公司
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