Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF8 Cites 1 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthesis method of 2-amino-4, 6-dihydroxypyrimidine

Examples

Experimental program
Comparison scheme
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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/545
CPCC07D239/545
Inventor 张赟许胜金标
Owner NANTONG TENDENCI CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com