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Synthetic method for 4,6-dichloropyrimidine

A technology of dichloropyrimidine and a synthesis method, applied in directions such as organic chemistry, can solve the problems of large amount of catalyst, high cost, cumbersome recovery and reuse process of organic bases, etc., and achieves avoiding recovery and reuse, low cost, and catalyst amount. small effect

Inactive Publication Date: 2018-07-31
CHONGQING UNISPLENDOUR CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of this, the purpose of the present invention is to provide a synthetic method of 4,6-dichloropyrimidine, which is used to solve the problems of complex recovery and reuse process of organic bases, large amount of catalyst and high cost in the prior art.

Method used

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  • Synthetic method for 4,6-dichloropyrimidine
  • Synthetic method for 4,6-dichloropyrimidine

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 212g of triphosgene (content 99%, 0.71mol) was dissolved in 500mL of nitrobenzene for use.

[0029] In the device equipped with reflux condenser, thermometer, stirrer and constant pressure dropping funnel, add 4,6-dihydroxypyrimidine (114g, content 98%, 1mol), triphenylphosphine oxide (8.4g, content 99 %, 0.03mol), cobalt phthalocyanine (0.57g, 0.001mol), stir and mix evenly, heat up to 90-95°C, and add dropwise a nitrobenzene solution of triphosgene to react.

[0030] Sampling and analysis after 5 hours of reaction, HPLC analysis showed that the content of 4,6-dihydroxypyrimidine was 0.25%, and the content of 4,6-dichloropyrimidine was 98.2%. degree-0.095Mpa), to obtain 4,6-dichloropyrimidine 143.8g (content 99.7%), yield 96.2% (based on 4,6-dihydroxypyrimidine).

Embodiment 2

[0040]In a device equipped with a reflux condenser, a thermometer, a stirrer and a constant pressure dropping funnel, add 4,6-dihydroxypyrimidine (114g, content 98%, 1mol), tri-n-octylphosphine oxide (7.74g, content 99%, 0.02mol), cobalt phthalocyanine (0.46g, 0.0008mol), stir and mix evenly, heat up to 110-120°C, add 297g of diphosgene (content 99%, 1.5mol) dropwise for reaction.

[0041] Sampling and analysis after 6 hours of reaction, HPLC analysis showed that the content of 4,6-dihydroxypyrimidine was 0.31%, and the content of 4,6-dichloropyrimidine was 97.5%. Degree -0.095Mpa), to obtain 4,6-dichloropyrimidine 141.6g (content 99.8%), yield 94.8% (calculated as 4,6-dihydroxypyrimidine).

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Abstract

The invention discloses a synthetic method for 4,6-dichloropyrimidine. The synthetic method comprises the following steps: (1) mixing 4,6-dihydroxypyrimidine with a catalyst, adding one or two selected from a group consisting of diphosgene and triphosgene, and carrying out a reaction; and (2) after the reaction is completed, separating and purifying a reaction solution so as to obtain the product4,6-dichloropyrimidine. The catalyst is a compound of organic phosphine and cobalt phthalocyanine. The synthetic method of the invention does not use any organic alkali, avoids the cumbersome processof recovery and recycling of the organic alkali, prevents the waste of resources and product loss, and is friendly to environment and free of additional solid waste and considerable phosphorus-containing waste liquid and waste residues; and a specific catalyst combination is used in the invention, the usage amount of the catalyst is small, and cost is low.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a synthesis method of 4,6-dichloropyrimidine. Background technique [0002] Pyrimidine compounds have active molecular structures and are intermediates of many medicines and pesticides. Because of their important role in the field of pesticides and medicine, they have attracted the attention of many scholars. When used as a pharmaceutical intermediate, it is mainly used in the production of sulfa drugs, such as sulfamethazine, sulfamethiadiazole, sulfamotosine, sulfa-6-methoxine, etc. 4,6-dichloropyrimidine is also an important intermediate for the synthesis of sulfonamides and the fungicide azoxystrobin. [0003] There have been many reports in the literature on its preparation methods. The most common method is: react 4,6-dihydroxypyrimidine with tertiary amines such as triethylamine, pyridine, N,N-dimethylaniline, and phosphorus oxychloride at a certain temperature...

Claims

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Application Information

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IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 丁永良张飞陈孝建钟显威陈依柔
Owner CHONGQING UNISPLENDOUR CHEM
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