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Preparation method of 4,6-dihydroxypyrimidine

The technology of dihydroxypyrimidine and hydroxypyrimidine sodium salt is applied in the field of preparation of 4,6-dihydroxypyrimidine, which can solve the problems of large environmental protection pressure, increased waste water treatment cost and high cost, and achieves reduction of environmental protection pressure and acid consumption. effect of reducing salt content

Inactive Publication Date: 2017-06-23
CHONGQING UNISPLENDOUR INT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the preparation process of the prior art, a large amount of acid solution needs to be consumed during acidification, and the cost is relatively high. At the same time, a large amount of saline wastewater is generated during the preparation process, causing greater environmental pressure and increasing the cost of wastewater treatment.

Method used

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Examples

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preparation example Construction

[0018] The invention provides a kind of preparation method of 4,6-dihydroxypyrimidine, comprising the following steps:

[0019] A) providing a 4,6-dihydroxypyrimidine reaction solution, using a bipolar membrane to treat the 4,6-dihydroxypyrimidine reaction solution to obtain a bipolar membrane treatment solution;

[0020] B) Acidifying the bipolar membrane treatment solution to obtain 4,6-dihydroxypyrimidine.

[0021] In the preparation method of 4,6-dihydroxypyrimidine provided by the present invention, before acidifying the 4,6-dihydroxypyrimidine reaction solution, a bipolar membrane is used for treatment in advance, which can reduce the amount of waste water and the salt content of waste water, and acidify It can significantly reduce the acid consumption, greatly reducing the cost and environmental protection pressure.

[0022] According to the present invention, a 4,6-dihydroxypyrimidine reaction solution is first provided, and a bipolar membrane is used to treat the 4,6...

Embodiment 1

[0038]Mix 80.0g dimethyl malonate and 60.0g formamide, add excess sodium methoxide methanol solution at 100°C, keep warm for 1h after adding, to obtain 4,6-dihydroxypyrimidine sodium salt mixture; then cool down to 70°C Concentrate the methanol and add water to continue the concentration; then add water to dissolve the 4,6-dihydroxypyrimidine sodium salt mixture to form a 4,6-dihydroxypyrimidine reaction solution. Utilize bipolar membrane to it process, until the pH of bipolar membrane treatment solution is 9.0; Under 40 ℃, be 37% hydrochloric acid to gained bipolar membrane treatment solution acidification with 131.9g mass concentration, be 2.5 to solution pH, then The resulting acidified solution was suction-filtered and dried to obtain 55.9 g of 4,6-dihydroxypyrimidine product. After testing, the purity of the obtained product was 98.2%, and the yield was 82.1%.

Embodiment 2

[0040] Mix 83.9g dimethyl malonate and 62.9g formamide, add excess sodium methoxide methanol solution at 95°C, keep warm for 1h after adding, to obtain 4,6-dihydroxypyrimidine sodium salt mixture; then cool down to 70°C Concentrate the methanol and add water to continue the concentration; then add water to dissolve the 4,6-dihydroxypyrimidine sodium salt mixture to form a 4,6-dihydroxypyrimidine reaction solution. Utilize bipolar membrane to it process, until the pH of bipolar membrane treatment solution is 10; Under 35 ℃, be 37% hydrochloric acid to gained bipolar membrane treatment solution acidification with 119.2g mass concentration, be 2.8 to solution pH, then The resulting acidified solution was suction filtered and dried to obtain 59.0 g of 4,6-dihydroxypyrimidine product. After testing, the obtained product has a purity of 98.5% and a yield of 82.5%.

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Abstract

The invention provides a preparation method of 4,6-dihydroxypyrimidine. A bipolar membrane is applied to a preparation process of 4,6-dihydroxypyrimidine; 4,6-dihydroxypyrimidine reaction liquid formed in a preparation process of 4,6-dihydroxypyrimidine is treated by the bipolar membrane in advance before an acidification technology; during acidification, the consumption of acid liquid can be reduced obviously; besides, the wastewater quantity and a salt content in wastewater are also reduced, so that the environmental protection pressure is reduced; and the wastewater treatment cost is reduced.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 4,6-dihydroxypyrimidine. Background technique [0002] 4,6-dihydroxypyrimidine is usually used as a fine chemical raw material or an intermediate in organic synthesis, and is widely used in the preparation of medicines, pesticides and fungicides. 4 , intermediates of antineoplastic drugs and auxiliary drugs; in addition, it can also be used to synthesize intermediates of methoxyacrylate fungicides, etc. Therefore, 4,6-dihydroxypyrimidine has a large market demand, and the preparation of 4,6-dihydroxypyrimidine is of great significance. [0003] In the prior art, 4,6-dihydroxypyrimidine is usually prepared in the following ways: (1) using malonate (such as diethyl malonate, or dimethyl malonate, etc.) and formamide as raw materials , form 4,6-dihydroxypyrimidine sodium salt under the action of alkali metal sodium alkoxide (such as sodium methoxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/54
CPCC07D239/54
Inventor 张飞丁永良钟显威陈伊柔陈孝建张兰
Owner CHONGQING UNISPLENDOUR INT CHEM