Synthesis method of 2-amino-4, 6-dihydroxypyrimidine

A technology of dihydroxypyrimidine and amino group is applied in the field of synthesizing 2-amino-4,6-dihydroxypyrimidine, which can solve problems such as low yield and achieve the effects of improving purity, preventing decomposition and wide application prospect.

Inactive Publication Date: 2016-11-30
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The productive rate of this preparation method is low, only about 70%

Method used

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  • Synthesis method of 2-amino-4, 6-dihydroxypyrimidine

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The method for synthesizing 2-amino-4,6-dihydroxypyrimidine in this example uses guanidine nitrate and diethyl malonate as raw materials for a one-step cyclization reaction. The specific steps of the synthesis method are as follows:

[0020] (1) Add 1.1 mol of 99% NaOH solid to 1 mol of 98% ethanol solution, and add 0.3 mol of 99% benzene to carry out azeotropic distillation to remove water, and finally remove Benzene, the sodium ethylate solution that obtains molar concentration is 2.8mol / L;

[0021] (2) Heat 1 mol of ammonium nitrate with a mass percentage concentration of 99% and 1.5 mol of dicyandiamide with a mass percentage concentration of 99% to a molten state, and then feed in liquid ammonia with a mass percentage concentration of 99%. Down heat preservation reaction, the temperature of heat preservation reaction is 200 ℃, and the reaction time is 30min, makes guanidine nitrate;

[0022] (3) Put 150 mL of 2.8 mol / L sodium ethoxide solution, 0.17 mol of 6.54 mo...

Embodiment 2

[0025] The method for synthesizing 2-amino-4,6-dihydroxypyrimidine in this example uses guanidine nitrate and diethyl malonate as raw materials for a one-step cyclization reaction. The specific steps of the synthesis method are as follows:

[0026] (1) Add 1.1 mol of 99% NaOH solid to 1 mol of 98% ethanol solution, and add 0.3 mol of 99% benzene to carry out azeotropic distillation to remove water, and finally remove Benzene, the sodium ethylate solution that obtains molar concentration is 2.8mol / L;

[0027] (2) Heat 1 mol of ammonium nitrate with a mass percentage concentration of 99% and 1.5 mol of dicyandiamide with a mass percentage concentration of 99% to a molten state, and then feed in liquid ammonia with a mass percentage concentration of 99%. Down heat preservation reaction, the temperature of heat preservation reaction is 180 ℃, and the reaction time is 45min, makes guanidine nitrate;

[0028] (3) Put 150 mL of 2.8 mol / L sodium ethoxide solution, 0.17 mol of 6.54 mo...

Embodiment 3

[0031] The method for synthesizing 2-amino-4,6-dihydroxypyrimidine in this example uses guanidine nitrate and diethyl malonate as raw materials for a one-step cyclization reaction. The specific steps of the synthesis method are as follows:

[0032] (1) Add 1.1 mol of 99% NaOH solid to 1 mol of 98% ethanol solution, and add 0.3 mol of 99% benzene to carry out azeotropic distillation to remove water, and finally remove Benzene, the sodium ethylate solution that obtains molar concentration is 2.8mol / L;

[0033] (2) Heat 1 mol of ammonium nitrate with a mass percentage concentration of 99% and 1.5 mol of dicyandiamide with a mass percentage concentration of 99% to a molten state, and then feed in liquid ammonia with a mass percentage concentration of 99%. Down heat preservation reaction, the temperature of heat preservation reaction is 190 ℃, and the reaction time is 38min, makes guanidine nitrate;

[0034] (3) Put 150 mL of 2.8 mol / L sodium ethoxide solution, 0.17 mol of 6.54 mo...

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Abstract

The invention relates to a synthesis method of 2-amino-4, 6-dihydroxypyrimidine. Guanidine nitrate and diethyl malonate are employed as the raw materials for one-step cyclization reaction. The steps include: employing a new-made sodium ethoxide solution, diethyl malonate and self-made guanidine nitrate to carry out stirring reflux reaction for 0.5-1.5h, distilling off ethanol, then dissolving the obtained white solid in water, then using a 4-6% acetic acid solution to conduct acidification to a pH value of 4-6, and carrying out filtering, washing and drying, thus obtaining a white solid 2-amino-4, 6-dihydroxypyrimidine. The method provided by the invention has the advantages of simple reaction steps, low reaction temperature, safety and environmental protection, is suitable for industrial production, and has wide application prospect.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for synthesizing 2-amino-4,6-dihydroxypyrimidine. Background technique [0002] 2-Amino-4,6-dihydroxypyrimidine is a pesticide intermediate used in the synthesis of sulfonylurea pesticides, such as bensulfuron-methyl, nicosulfuron-methyl, cyprosulfuron-methyl, ethoxysulfuron-methyl, sulfarimsulfuron sulfuron, sulfuron-methyl, pyrazosulfuron-methyl, chlorpyrazosulfuron-methyl, rimsulfuron-methyl tetrazole, pyrazosulfuron-methyl (NC-311), etc. [0003] The existing preparation method is to add sodium ethylate and diethyl malonate in the reactor, then add guanidine nitrate, stir, and heat to reflux for 7 h, cool to room temperature and discharge, the filtrate is distilled to recover absolute ethanol, and Put the cake into the washing kettle again, add water and stir, heat to 80°C, after it is completely dissolved, slowly add concentrated hydrochloric acid, adjust the pH va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/545
CPCC07D239/545
Inventor 张赟许胜金标
Owner NANTONG TENDENCI CHEM
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