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Method for preparing 2-amino-4, 6-dimethoxypyrimidine

A technology of dimethoxypyrimidine and dimethyl cyanomalonimide, which is applied in organic chemistry and other fields, can solve problems such as high cost of malononitrile, easy decomposition and polymerization, and unstable temperature, and achieve less waste , simple operation, easy solvent effect

Active Publication Date: 2013-06-19
HUBEI HUIDA HIGH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But due to the high cost of malononitrile, intermediate dimethoxymalonamidine hydrochloride and substituted cyanamide acid-base and unstable temperature, problems such as easy decomposition and polymerization, so the route has lower yield and lower cost at present. High and harsh operating conditions, but this method has simple steps and less waste, and is worth exploring in today's increasingly demanding environmental protection

Method used

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  • Method for preparing 2-amino-4, 6-dimethoxypyrimidine
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  • Method for preparing 2-amino-4, 6-dimethoxypyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Synthesis of Dimethoxypropanediamidine (ADMP01)

[0039]At room temperature, add malononitrile (132.0g / 2.0mol) methanol solution (1000ml) and solid titanium tetrachloride (2.6g) into a 2L four-neck flask, stir and mix well, pass dry hydrogen chloride into the system Gas, keep the pressure of 0.1 ~ 0.5MPa, heat the reaction at 25 ~ 35 ℃ and stir for 4 hours, stop the reaction, degas, filter, and obtain the solution of dimethoxypropanediamidine, which can be directly used in the next reaction.

[0040] (2) Synthesis of Dimethyl Cyanomalonimide (ADMP02)

[0041] Add 600ml of buffer solution prepared by mixing disodium hydrogen phosphate (71.0g / 0.5mol) and sodium bicarbonate (25.2g / 0.3mol) into a 2L four-neck flask, stir, cool down to below 0°C in an ice-salt bath, add 50 % NH 2 CN aqueous solution (214.2g / 2.55mol), add the solution of dimethoxypropanediamidine (ADMP01), the pH value of the reaction solution is maintained at 8~9 during the dropwise addition, after the...

Embodiment 2

[0046] (1) Synthesis of Dimethoxypropanediamidine (ADMP01)

[0047] Add malononitrile (132.0g / 2.0mol) and methyl acetate solution (1000ml) of methanol (320.0g / 10.0mol) and zirconia (3.0g) into a 2L four-necked flask, cool to 0~ Stir and mix well at 10°C, pass dry hydrogen chloride gas into the system, keep the pressure of 0.1~0.5MPa, stir for 7 hours, stop the reaction, degas, filter, and obtain the solution of dimethoxypropanediamidine, which can be used directly react in the next step.

[0048] (2) Synthesis of Dimethyl Cyanomalonimide (ADMP02)

[0049] Add 600ml of buffer solution prepared by disodium hydrogen phosphate (28.4g / 0.2mol) and ammonium bicarbonate (39.5g / 0.5mol) into a 2L four-neck flask, stir, cool down in an ice-salt bath to below 0°C, add 50% NH 2 CN aqueous solution (214.2g / 2.55mol), add the solution of dimethoxypropanediamidine (ADMP01), the pH value of the reaction solution is maintained at 8~9 during the dropwise addition process, after the addition is...

Embodiment 3

[0054] (1) Synthesis of Dimethoxypropanediamidine (ADMP01)

[0055] At room temperature, add malononitrile (132.0g / 2.0mol) and methyl tert-butyl ether solution (1000ml) and cobalt chloride (1.5g) of methanol (320.0g / 10.0mol) in a 2L four-necked flask, Stir and mix well, pass dry hydrogen chloride gas into the system, keep the pressure of 0.1-0.5MPa, keep warm at 25-35°C and stir for 4 hours, stop the reaction, degas, filter, and obtain the solution of dimethoxypropanediamidine , which can be directly used in the next reaction.

[0056] (2) Synthesis of Dimethyl Cyanomalonimide (ADMP02)

[0057] Add 3% ammonia water (566.7g / 1.0mol) into a 2L four-neck flask, cool down in an ice-salt bath to below 0°C, add 50% NH 2 CN aqueous solution (214.2g / 2.55mol), add the solution of dimethoxypropanediamidine (ADMP01), and control the feeding speed by detecting the pH value of the system. During the dropping process, the pH value of the reaction solution is maintained at 8-9. After the a...

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Abstract

The present invention relates to a method for preparing 2-amino-4, 6-dimethoxypyrimidine (ADMP). According to the method, malononitrile is uses as a raw material, special solvents are adopted, and in the action of a specific catalyst, after reactions of imidization, cyanamide substitution, aromatic cyclization, etc., 2-amino-4, 6-dimethoxypyrimidine of high purity is synthesized in a high yield. The method has no harsh conditions in all the steps, is simple in operation, little in the amounts of waste water, waste gas and industrial residues, and environmentally friendly, thereby having significant social and economic benefits, and being suitable for industrial production.

Description

technical field [0001] The present invention relates to the preparation method and production process of 2-amino-4,6-dimethoxypyrimidine (ADMP), an important intermediate of medicine and pesticide. The method of the present invention uses malononitrile as raw material, adopts special solvent, and Under the action of a catalyst, 2-amino-4,6-dimethoxypyrimidine is synthesized through reactions such as imidization, cyanamide substitution, and aromatic ring closure. The purity of the product is greater than 99%, and the highest total yield reaches more than 77%. The preparation method of the invention has the characteristics of cheap and easy-to-obtain raw materials, no harsh conditions for reaction, simple operation, less three wastes, environmental friendliness and the like, and is suitable for industrial production. Background technique [0002] Pyrimidine compounds are a class of important biologically active substances, which are widely used in insecticides, herbicides, fun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/52
Inventor 凌云李永芳吴清来陈立柱殷巍
Owner HUBEI HUIDA HIGH TECH CO LTD
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