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Synthetic method of piribedil

A technology for piribedil and piperazine, applied in the field of synthesizing piribedil, can solve the problems of complicated operation, unfavorable industrialization, difficult industrialization, etc., and achieve the effects of simplifying synthesis steps, improving utilization rate, and reducing the generation of three wastes

Active Publication Date: 2017-02-22
SUZHOU HOMESUN PHARMA
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Problems solved by technology

Using cyanoborohydride reduction, the yield can reach 60%, but the operation is cumbersome, the purification is difficult, and ion exchange chromatography is required for purification, which is not conducive to industrialization
[0007] 3 Using piperazine pyrimidine as raw material, piribedil was prepared by direct alkylation reaction with piperonyl alcohol under the action of ruthenium catalyst, but the raw material cost is too high to be industrialized
The yield of the second step of the literature is difficult to repeat, while the yield of the third step of the literature is only 68%.

Method used

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  • Synthetic method of piribedil
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  • Synthetic method of piribedil

Examples

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Embodiment Construction

[0025] Reaction example 1 (Chinese patent 1884280)

[0026] 1 Preparation of piperonyl piperazine

[0027] Add 39.2g piperonal, 34.4g piperazine, 400ml methyl tert-butyl ether and 7g10% palladium charcoal catalyst in the high-pressure hydrogenation reactor, replace the air with hydrogen for 3 times after nitrogen replacement air 3 times, under 10kg hydrogen pressure, Heat the reaction at 50~60°C for 15~20 hours, lower the temperature, filter the catalyst, cool the filtrate to 13~18°C, filter the precipitated piperazine, add 150ml of water to the filtrate, keep it warm at 13~18°C, adjust the pH to 7.9~ with 7N hydrochloric acid 8.0. Separate the liquid, extract the water phase with toluene 3 times, combine the water phases, adjust the pH to 12 with 20 g of sodium hydroxide under ice bath, extract again with toluene 3 times, combine the organic phases, dry and filter with anhydrous magnesium sulfate, and concentrate to obtain 45 g Pale yellow viscous substance, yield 78%.

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Abstract

The invention relates to a synthetic method of piribedil. The synthetic method is a brand new process comprising the steps of synthesizing piperonyl piperazine in one step under the effects of pentamethyleneamine, piperazine pyrimidine and paraformaldehyde, and reacting by virtue of piperonyl piperazine and dichloropyrimidine so as to synthesize piribedil. Piperonyl piperazine has not been synthesized by virtue of the synthetic method before. Compared with a traditional synthetic method of piribedil, the synthetic method has the advantages that synthetic steps are simplified, the three wastes are reduced, the utilization ratio of pentamethyleneamine is remarkably increased, and the after-treatment is relatively environment-friendly.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing piribedil. Background technique [0002] The chemical name of piribedil is 2-[4-(3,4methylenedioxybenzyl)]piperazin-1-ylpyrimidine, a slow-release dopamine developed by Servier Pharmaceuticals in France receptor agonists. It acts on D2 and D3 receptors, restores the balance between acetylcholine and dopamine systems by increasing the excitability of dopamine receptors, and is clinically used for the treatment of Parkinson's disease (PD). The combination of piribedil and levodopa can not only improve the motor function of early PD patients, but also significantly reduce the dyskinesia caused by levodopa treatment. Compared with levodopa, the use of dopamine agonists has fewer motor complications. [0003] Le ebrun et al. compared bromocriptine, ropinirole, pergolide, pramipexole, and piribel, and believed that piribedil has strong selectivity and can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/12
CPCC07D405/12
Inventor 翟金星樊超陆红彬
Owner SUZHOU HOMESUN PHARMA
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