Synthetic method of 2-formic acid-3-propoxyl-5-methylpyrrole

A technology of methylpyrrole and synthesis method, applied in the direction of organic chemistry, etc., can solve the problems of poor solubility, limitation, harsh synthesis conditions, etc.

Inactive Publication Date: 2016-07-27
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because triphenylamine compounds generally have small molecular weight, poor solubility, and harsh synthesis conditions, they are subject to many restrictions in practical application.

Method used

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  • Synthetic method of 2-formic acid-3-propoxyl-5-methylpyrrole

Examples

Experimental program
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example 1

[0015] Add 40mL of ethyl acetate to a 500mL three-necked flask equipped with a thermometer, add 40mL of 1-propanol and 200mL of absolute ethanol into the flask, put it into an ice bath with stirring at 500r / min and cool to -8°C, and keep it Slowly add 20 mL of potassium hydroxide solution with a mass fraction of 25% at high temperature into the flask, continue to stir for 1 hour after the addition, perform suction filtration to remove the organic solvent after the reaction is completed, and wash the filter residue twice with ether before suction filtration and drying. Obtain light yellow solid, namely potassium 4-oxo-2-penten-2-alcohol; add 3 g of above-mentioned potassium 4-oxo-2-penten-2-alkolate in a 250mL three-necked flask, add to it Mix 15mL of 35% nitric acid solution and 30mL of distilled water, mix and stir evenly, pass nitrogen gas into the three-necked flask, and stir for 20 minutes, then stop the flow, heat the temperature to 70°C, add 3g of acetamidopropanediol to ...

example 2

[0017] Add 55mL of ethyl acetate to a 500mL three-necked flask equipped with a thermometer, add 50mL of 1-propanol and 200mL of absolute ethanol into the flask, and put it into an ice bath with stirring at 550r / min to cool to -6°C and keep at this temperature Slowly add 23 mL of potassium hydroxide solution with a mass fraction of 25% into the flask, continue to stir for 1 hour after the addition, and remove the organic solvent by suction filtration after the reaction is completed. Pale yellow solid, which is potassium 4-oxo-2-penten-2-alcohol; add 3.5 g of potassium 4-oxo-2-penten-2-alcohol obtained above into a 250 mL three-necked flask, and add to it 17mL of 35% nitric acid solution and 35mL of distilled water were mixed and stirred evenly, and nitrogen gas was introduced into the three-necked flask, and the reaction was stirred for 25 minutes. Acetate diethyl ester and 13mL of distilled water, while continuing to heat to 85°C for reflux, reflux reaction for 1.5h, after the...

example 3

[0019]Add 70mL of ethyl acetate to a 500mL three-neck flask equipped with a thermometer, add 60mL of 1-propanol and 200mL of absolute ethanol into the flask, put it into an ice bath with stirring at 600r / min, cool to -5°C, and keep at this temperature Slowly add 25 mL of potassium hydroxide solution with a mass fraction of 25% into the flask, continue to stir for 1 hour after the addition, and remove the organic solvent by suction filtration after the reaction is completed. Pale yellow solid, which is potassium 4-oxo-2-penten-2-alcohol; add 4 g of the above-mentioned potassium 4-oxo-2-penten-2-alcohol to a 250 mL three-necked flask, and add 30 mL of potassium 4-oxo-2-penten-2-alcohol Mass fraction 35% nitric acid solution and 40mL distilled water, after mixing and stirring evenly, pass nitrogen gas into the three-necked flask, and stir for 30 minutes, then stop the flow, heat the temperature to 75°C, and add 5g of acetamidomalonic acid into the bottle Diethyl ester and 15mL di...

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Abstract

The invention discloses a synthetic method of 2-formic acid-3-propoxyl-5-methylpyrrole, and belongs to the field of chemical synthesis.The method comprises the steps that ethyl acetate, 1-propyl alcohol, absolute ethyl alcohol and a potassium hydroxide solution with the mass fraction of 25% are reacted to obtain 4-oxo-2-amylene-2-potassium alcoholate, the product is mixed with a salpeter solution and distilled water, diethyl acetamidomalonate is added for backflow, then ice water is added, and a large amount of solid, namely 2-ethyl formate-3-propoxyl-5-methylpyrrole is generated; then a copper oxide solution is added, suction filtering is carried out after stirring, sulfuric acid is added into the filtrate, precipitation is produced, 2-ethyl formate-3-propoxyl-5-methoxylpyrrole is obtained, alkali is used for hydrolysis, and therefore the 2-formic acid-3-propoxyl-5-methylpyrrole is obtained.

Description

technical field [0001] The invention discloses a synthesis method of 2-formic acid-3-propoxy-5-methylpyrrole, which belongs to the field of chemical synthesis. Background technique [0002] In the development process of energetic materials, energy and safety have always been a pair of contradictions that are difficult to reconcile. For many years, people have been looking for new elemental explosives with better safety and higher energy. [0003] In recent years, experts in energetic materials have made great progress in synthesis, and have synthesized a series of materials with higher energy than 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) and similar safety. Based on TATB's single-substance explosives, it provides more alternative new single-substance explosives for the formulation design of plastic bonded explosives (PBX). 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105) is a new type of insensitive high-energy explosive with excellent comprehensive properties, which i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/36
CPCC07D207/36
Inventor 陈兴权
Owner CHANGZHOU UNIV
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