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Method for synthesizing 1-(2-pyrimidine) piperazine

A synthesis method and pyrimidine-based technology are applied in the synthesis field of 1-piperazine, can solve the problem of high production cost, and achieve the effects of low production cost and improved reaction yield

Active Publication Date: 2010-06-02
太仓市茜泾化工有限公司
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Problems solved by technology

The prior art kind mainly adopts the condensation reaction of piperazine and 2-chloropyrimidine to synthesize 1-(2-pyrimidinyl) piperazine under alkaline conditions, and the reaction uses chloroform as solvent, and the yield (mole) is only about 50%. high production cost

Method used

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Examples

Experimental program
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Embodiment Construction

[0011] The specific embodiment of the present invention is described below:

[0012] Into a 1L four-necked flask, add 100g~120g of anhydrous piperazine, 60g~70g of anhydrous sodium carbonate, 500ml of water, 1~2g of butyltriphenylphosphine bromide, stir and heat, and add in batches at 40~60°C After adding 58g (0.5mol) of 2-chloropyrimidine, continue stirring for 1 hour, and then slowly cool to 25-30°C. The white 1,4-bis(2-pyrimidine)piperazine by-product was removed by filtration, and the filtrate was retained.

[0013] The above-mentioned filtrate was extracted with chloroform, the amount of chloroform was 250ml each time, and the extraction was 2-3 times in total. The chloroform layer was dried with anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under normal pressure to recover the solvent, then concentrated under reduced pressure until the chloroform was evaporated, then changed to high vacuum, and the temperature was raised slowly, and the fracti...

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Abstract

The invention relates to a synthesis method of 1-(2-pyrimidine) piperazine, which comprises at alkali condition and in the presence of phase transfer catalyst, condensing piperazine and 2-chloro pyrimidine to obtain 1-(2-pyrimidine) piperazin, wherein the solvent of the condensation reaction is water or the mixture of water and organic solvent. The synthesis method has low production cost.

Description

technical field [0001] The invention relates to a synthesis method of 1-(2-pyrimidinyl)piperazine. Background technique [0002] 1-(2-pyrimidinyl)piperazine, also known as 2-pyrimidinepiperazine, is an intermediate of a new type of azaspirodecane diketone anxiolytic drug, and is currently mainly used in the production of the antidepressant buspirone. The prior art kind mainly adopts the condensation reaction of piperazine and 2-chloropyrimidine to synthesize 1-(2-pyrimidinyl) piperazine under alkaline conditions, and the reaction uses chloroform as solvent, and the yield (mole) is only about 50%. Production costs are high. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a synthetic method of 1-(2-pyrimidinyl)piperazine in order to overcome the deficiencies of the prior art. The yield of the method is greater than 80%, and the production cost is low. [0004] In order to achieve the above object, the technical s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D403/04B01J31/02
Inventor 秦正浩
Owner 太仓市茜泾化工有限公司
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